KR100556903B1 - Method for preparing inorganic binder using liquid sodium silicate - Google Patents
Method for preparing inorganic binder using liquid sodium silicate Download PDFInfo
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- KR100556903B1 KR100556903B1 KR1020050046874A KR20050046874A KR100556903B1 KR 100556903 B1 KR100556903 B1 KR 100556903B1 KR 1020050046874 A KR1020050046874 A KR 1020050046874A KR 20050046874 A KR20050046874 A KR 20050046874A KR 100556903 B1 KR100556903 B1 KR 100556903B1
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- sodium silicate
- inorganic binder
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- liquid sodium
- water
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- 239000011230 binding agent Substances 0.000 title claims abstract description 78
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000004115 Sodium Silicate Substances 0.000 title claims abstract description 57
- 229910052911 sodium silicate Inorganic materials 0.000 title claims abstract description 57
- 239000007788 liquid Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- -1 sodium inorganic acid Chemical class 0.000 claims abstract description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 30
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 21
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 159000000000 sodium salts Chemical class 0.000 claims description 10
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims 2
- 150000001340 alkali metals Chemical class 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 abstract description 17
- 239000003795 chemical substances by application Substances 0.000 abstract description 11
- 229910052708 sodium Inorganic materials 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 7
- 229910052784 alkaline earth metal Inorganic materials 0.000 abstract description 6
- 150000001342 alkaline earth metals Chemical class 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 230000003578 releasing effect Effects 0.000 abstract description 2
- 229940032158 sodium silicate Drugs 0.000 description 48
- 235000019794 sodium silicate Nutrition 0.000 description 48
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000005452 bending Methods 0.000 description 16
- 239000008188 pellet Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 229920006395 saturated elastomer Polymers 0.000 description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 239000000853 adhesive Substances 0.000 description 10
- 230000001070 adhesive effect Effects 0.000 description 10
- 238000010828 elution Methods 0.000 description 9
- 229910001629 magnesium chloride Inorganic materials 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 229910001948 sodium oxide Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000010451 perlite Substances 0.000 description 2
- 235000019362 perlite Nutrition 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- CZIMGECIMULZMS-UHFFFAOYSA-N [W].[Na] Chemical compound [W].[Na] CZIMGECIMULZMS-UHFFFAOYSA-N 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- FZFYOUJTOSBFPQ-UHFFFAOYSA-M dipotassium;hydroxide Chemical compound [OH-].[K+].[K+] FZFYOUJTOSBFPQ-UHFFFAOYSA-M 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators or shrinkage compensating agents
- C04B22/002—Water
- C04B22/004—Water containing dissolved additives or active agents, i.e. aqueous solutions used as gauging water
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators or shrinkage compensating agents
- C04B22/08—Acids or salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
본 발명은 액상 규산소다를 이용한 무기 바인더의 제조방법에 관한 것으로, 좀 더 상세하게는 액상 규산소다에 일정량의 염산을 첨가·교반하여 무기산 나트륨을 결정화시킴으로써 대기 중의 수분이나 물에 대한 풀어짐 현상이 없는 내수성이 강한 무기 바인더의 제조가 가능하며, 제조장치가 간단하고 공정이 단순하여 전체적인 제조비용을 절감할 수 있고, 인체 및 환경에 유해한 유기용제를 사용하지 않아 환경친화적인 액상 규산소다를 이용한 무기바인더의 제조방법에 관한 것이다.The present invention relates to a method for producing an inorganic binder using liquid sodium silicate, and more particularly, by adding and stirring a certain amount of hydrochloric acid to liquid sodium silicate to crystallize sodium inorganic acid, there is no releasing effect on water or water in the air. Inorganic binders with strong water resistance can be manufactured, and the manufacturing apparatus is simple and the process is simple, which can reduce the overall manufacturing cost, and does not use organic solvents that are harmful to humans and the environment. It relates to a manufacturing method of.
액상 규산소다, 염산, 알카리토금속, 무기 바인더, 그라우팅제 Liquid sodium silicate, hydrochloric acid, alkaline earth metal, inorganic binder, grouting agent
Description
본 발명은 액상 규산소다를 이용한 무기 바인더의 제조방법에 관한 것으로, 좀 더 상세하게는 액상 규산소다에 산용액으로 염산을 일정배율로 첨가하여 나트륨염을 생성함으로써 수분에 대하여 안정성을 갖는 액상 규산소다를 이용한 무기 바인더의 제조방법에 관한 것이다.The present invention relates to a method for producing an inorganic binder using liquid sodium silicate, and more particularly, to liquid sodium silicate, which is a liquid sodium silicate having stability against water by adding hydrochloric acid in a predetermined ratio to an acid solution to generate sodium salt. It relates to a method for producing an inorganic binder using.
일반적으로 규산소다는 Na2O와 SiO2의 결합비율에 따라 소디윰 메타실리카(sodium metasillica), 세스퀴 실리케이트(sesqui-sillicate), 오르소 실리케이트(ortho-sillicate) 등으로 불리우며, 현재 용도에 따라서 40여종 이상의 규산소다가 상품화되어 시판되고 있다. In general, sodium silicate is called sodium metasillica, sesqui-sillicate, ortho-sillicate, etc., depending on the ratio of Na 2 O to SiO 2 . More than 40 kinds of sodium silicate have been commercialized and marketed.
특히, 물유리라 불리는 액상 규산소다는 점성질의 알칼리성을 나타내는 투명한 용액으로, 한국공업규격(KS M 1415)에서 정하는 액상 규산소다의 몰비는 Na2O와 SiO2에 대하여 1 : 2.064 ~ 4.300으로 여러가지 조성을 갖는다.In particular, liquid sodium silicate, called water glass, is a viscous alkaline solution. The molar ratio of liquid sodium silicate in Korean Industrial Standard (KS M 1415) is 1: 2.064 ~ 4.300 for Na 2 O and SiO 2 . Has a composition.
이러한 액상 규산소다는 고유의 접착력을 가지고 있어서 접착제나 연약지반 을 개량하기 위한 그라우팅제로 이용되고 있는데, 다른 접착제나 그라우팅제보다 제조공정이 단순하고 설비가 간단할 뿐만 아니라 생산비용이 저렴하여 널리 이용되고 있다. 특히 제조공정 전, 후 및 사용시에 유기 접착제와 달리 공해를 유발시키지 않는다는 장점을 가지고 있어 환경친화적인 면에서 각광을 받고 있다.This liquid sodium silicate is used as a grouting agent to improve adhesives or soft grounds because of its inherent adhesive strength, and it is widely used due to its simple manufacturing process, simple equipment, and low production cost than other adhesives and grouting agents. have. In particular, unlike the organic adhesives before, during and after the manufacturing process has the advantage that does not cause pollution has attracted the spotlight in terms of environmental friendliness.
그러나 접착제 또는 그라우팅제로 액상 규산소다를 이용할 경우, 규산소다에 포함된 나트륨 이온이 공기 중의 수분이나 물과 쉽게 반응하여 수산화나트륨과 같은 염을 형성하기 때문에 수분이나 물에 접촉되면 친수성으로 변화되어 수분에 의해 풀어짐 현상이 발생되고 강도가 저하되어 바인더로서의 역할을 수행하지 못하게 된다는 문제점이 발생된다.However, when liquid sodium silicate is used as an adhesive or grouting agent, sodium ions contained in sodium silicate easily react with water or water in the air to form salts such as sodium hydroxide. Thereby, a problem arises that the unwinding phenomenon occurs and the strength is lowered so that it cannot serve as a binder.
이와 같은 문제점 때문에 일부에서는 액상 규산소다에 카본 및 제올라이트를 첨가한 혼합 바인더를 사용하고 있으나, 액상 규산소다가 표면을 코팅함으로써 흡착능이 현저히 떨어지고 강도가 낮게 나타나며 물에 풀리는 현상이 개선되지 않아 바인더로 이용하는데는 여전히 어려움이 따르고 있다.Because of these problems, some of them use a mixed binder in which carbon and zeolite are added to the liquid sodium silicate. However, the liquid sodium silicate is coated as a surface, so that the adsorption capacity is significantly lowered and the strength is lowered. There are still difficulties.
따라서 본 발명은 상기와 같은 제반 문제점을 해결하기 위한 것으로, 액상 규산소다에 일정량의 염산을 첨가·교반하여 무기산 나트륨을 염으로 결정화시킴으로써 대기 중의 수분이나 물에 대하여 내성이 강하고, 제조장치가 간단하고 공정이 단순하여 제조비용을 절감할 수 있으며, 인체 및 환경에 유해한 유기용제를 사용하지 않아 환경친화적일 뿐만 아니라 접착제나 그라우팅제로 유용하게 사용할 수 있 는 액상 규산소다를 이용한 무기 바인더의 제조방법을 제공하는 것을 목적으로 한다.Accordingly, the present invention is to solve the above problems, by adding and stirring a certain amount of hydrochloric acid to the liquid sodium silicate to crystallize sodium inorganic acid with salt, which is resistant to moisture and water in the air, and the manufacturing apparatus is simple. The manufacturing process is simple and the manufacturing cost can be reduced, and it is not only environmentally friendly by using organic solvents that are harmful to human body and environment, but also provides a manufacturing method of inorganic binder using liquid sodium silicate which can be useful as an adhesive or grouting agent. It aims to do it.
상기와 같은 목적을 해결하기 위하여 본 발명은,The present invention to solve the above object,
온도는 20 ~ 40℃이고, 20 ~ 200RPM으로 회전하는 반응기에 액상 규산소다를 넣고 산용액을 서서히 첨가한 후, 1시간 동안 교반하여 결정화된 나트륨염을 포함한 규산물을 생성시키고, 물을 전체 무게에 대하여 20 ~ 30중량%가 되도록 첨가한 다음, 20 ~ 40℃에서 3시간 동안 교반하여 나트륨염을 용해시키고, 알카리토금속을 함유하는 화합물을 첨가하는 것을 포함하는 액상 규산소다를 이용한 무기 바인더의 제조방법에 있어서,Temperature is 20 ~ 40 ℃, liquid sodium silicate is added to the reactor rotating at 20 ~ 200RPM, acid solution is slowly added, and stirred for 1 hour to produce a siliceous product containing crystallized sodium salt, the total weight of water To prepare an inorganic binder using a liquid sodium silicate, which is added to 20 to 30% by weight, followed by stirring at 20 to 40 ° C. for 3 hours to dissolve sodium salts and adding a compound containing alkaline earth metal. In the method,
상기 액상 규산소다에 첨가되는 산용액이 포화농도의 염화수소 수용액(conc-HCl)이고, 상기 염화수소 수용액이 액상 규산소다에 포함되는 산화나트륨(Na2O)에 대하여 20 ~ 30중량%가 되도록 첨가하는 것을 특징으로 하는 액상 규산소다를 이용한 무기 바인더의 제조방법을 제공함으로써 달성될 수 있다.The acid solution added to the liquid sodium silicate is a saturated aqueous hydrogen chloride solution (conc-HCl), and the aqueous solution of hydrogen chloride is added so as to be 20 to 30% by weight relative to sodium oxide (Na 2 O) contained in the liquid sodium silicate. It can be achieved by providing a method for producing an inorganic binder using a liquid sodium silicate characterized in that.
이하에서는 본 발명에 대하여 좀 더 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
먼저, 20 ~ 200RPM으로 회전하는 반응기내에서 액상 규산소다에 산용액으로서 포화농도의 염화수소 수용액(conc-HCl)을 첨가하고 교반하게 되는데, 액상 규산소다가 삽입되어 있는 반응기에 포화농도의 염화수소 수용액(conc-HCl)을 서서히 첨가한 다음, 반응기내의 온도를 20 ~ 40℃를 유지하면서 1시간 동안 교반하게 되면 젤라틴상 또는 투명한 결정상의 규산물이 형성된다.First, a saturated aqueous hydrogen chloride solution (conc-HCl) is added to the liquid sodium silicate as an acid solution and stirred in a reactor rotating at 20 to 200 RPM, and a saturated hydrogen chloride aqueous solution ( After slowly adding conc-HCl), the mixture is stirred for 1 hour while maintaining the temperature in the reactor at 20 to 40 ° C. to form gelatinous or transparent crystalline silicate.
즉, 상기와 같은 반응을 통하여 결정상인 무기산 나트륨염을 생성시킴과 동시에 규산나트륨의 일부를 규산상태로 변형시킴으로써, 대기 중의 수분에 대해 흡착능을 갖는 나트륨 이온이 결정체인 나트륨염으로 변형되므로 제조되는 바인더는 수분에 의한 풀어짐 현상이 일어나지 않으며, 접착 후 장시간이 지나도 그 접착력이 떨어지지 않아 내수성에서 탁월한 효과를 갖게 된다.That is, a binder prepared by producing a sodium salt as an crystalline phase and transforming a part of sodium silicate into a silicic state through the above reaction, so that sodium ions having adsorption capacity to moisture in the air are transformed into crystalline sodium salt. The release phenomenon due to moisture does not occur, and even after a long time after the adhesion does not drop the adhesive force has an excellent effect in water resistance.
이때 액상 규산소다에 산화칼륨(K2O) 또는 산화리튬(Li2O)이 함유된 것을 사용하면 더욱 효과적인데, 이는 제조된 무기 바인더를 접착제나 그라우팅제로 사용하였을 경우 그 내수성이 더욱 향상될 수 있기 때문이다.At this time, it is more effective to use potassium oxide (K 2 O) or lithium oxide (Li 2 O) in the liquid sodium silicate, which can be improved even more when the prepared inorganic binder is used as an adhesive or grouting agent. Because there is.
이와 같은 액상 규산소다와 포화농도의 염화수소 수용액(conc-HCl)의 반응과정에 대하여 하기 반응식 1을 통해 좀 더 상세하게 설명하기로 한다.The reaction process of such a liquid sodium silicate and a saturated aqueous hydrogen chloride solution (conc-HCl) will be described in more detail through Scheme 1 below.
상기 반응식 1을 참고로 하여 산용액으로 포화농도의 염화수소 수용액(conc-HCl)을 사용한 경우를 살펴보면, 반응 후 생성물로서 이산화규소(SiO2)와 염화나트륨(NaCl), 물(H2O)을 각각 생성하게 되고, 염화나트륨은 결정체로 존재하므로 수분에 대하여 안정성을 갖게 된다.Referring to the case of using a saturated hydrogen chloride solution (conc-HCl) as an acid solution with reference to Scheme 1, after the reaction, silicon dioxide (SiO 2 ), sodium chloride (NaCl), water (H 2 O) as a product It is produced, and sodium chloride is present as crystals, so it is stable to moisture.
상기와 같이 산용액으로 염산을 사용하는 경우, 염화수소 수용액의 양은 액상 규산소다에 포함되는 산화나트륨(Na2O)에 대하여 20 ~ 30중량%를 첨가하는 것이 가장 효과적이며, 만약 염화수소 수용액의 양을 20중량% 미만으로 첨가하게 되면 규산소다로 부터 충분한 염화나트륨을 생성하지 못하므로 이온상태의 나트륨이 존재하여 제조되는 바인더의 수분에 대한 안정성이 떨어지게 되는 문제점이 발생된다. When hydrochloric acid is used as the acid solution as described above, it is most effective to add 20-30 wt% of the aqueous solution of hydrogen chloride based on sodium oxide (Na 2 O) contained in the liquid sodium silicate. When added to less than 20% by weight does not produce enough sodium chloride from the sodium silicate, there is a problem that the stability of the moisture of the binder produced due to the presence of ionic sodium occurs.
반대로 염화수소 수용액의 양을 30중량% 초과하여 첨가하게 되면 역시 반응 후 생성된 젤리상의 규산물이 후공정에서 용해되지 못하여 제품으로 생산이 어렵다는 문제점이 발생하기 때문이다. On the contrary, when the amount of the aqueous hydrogen chloride solution is added in excess of 30% by weight, it is also difficult to produce the product due to the inability to dissolve the silicate silicate produced in the subsequent process.
상기와 같이 규산소다에 산용액으로 포화농도의 염화수소 수용액을 첨가하고 교반하여 나트륨염을 포함한 규산물을 생성한 다음, 고체로 결정화된 나트륨염이 용해될 수 있도록 물을 전체 무게에 대하여 20 ~ 30중량%가 되도록 첨가하고, 20 ~ 40℃에서 3시간 동안 교반하여 결정체를 완전히 용해시키게 되면 수용액상의 무기 바인더가 제조된다.As described above, an aqueous solution of hydrogen chloride having a saturated concentration is added to the sodium silicate as an acid solution, followed by stirring to produce a siliceous product including sodium salt. Then, water is added to the total weight so as to dissolve the sodium salt crystallized as a solid. The solution is added in an amount of% by weight, and stirred at 20 to 40 ° C. for 3 hours to completely dissolve the crystals, thereby preparing an inorganic binder in an aqueous solution.
이와 같이 액상 규산소다와 염화수소 수용액의 반응이 종료된 시점에서 물을 첨가하여 수용액으로 만든 후 탄산칼슘(CaCO3), 질산칼슘(Ca(NO3)2), 염화마그네슘(MgCl2), 황산마그네슘(MgSO4), 수산화칼슘(Ca(OH)2)과 같은 알카리토금속을 함유하는 염, 산화물 및 수산화물 중에 하나를 선택하여 첨가하게 되면 좀 더 좋은 효과를 가져오게 되는데, 상기와 같은 알카리토금속을 함유하는 화합물은 바인더로 이용시 굽힘강도나 펠릿 타입(Pellet type) 강도 및 강제건조에 따른 표면균열 강도의 증가를 가져오기 때문이다. When the reaction of liquid sodium silicate and aqueous hydrogen chloride solution is completed, water is added to form an aqueous solution, followed by calcium carbonate (CaCO 3 ), calcium nitrate (Ca (NO 3 ) 2 ), magnesium chloride (MgCl 2 ), and magnesium sulfate (MgSO 4 ), salts, oxides and hydroxides containing alkali earth metals such as calcium hydroxide (Ca (OH) 2 ) is selected and added to bring a better effect, such as containing alkaline earth metals This is because the compound has an increase in the bending strength, pellet type strength and surface crack strength due to forced drying when used as a binder.
상기와 같이 첨가되는 알카리토금속을 함유하는 화합물은 제조된 무기 바인 더의 전체 무게에 대하여 0.1 ~ 0.5중량%가 되도록 첨가하는 것이 적절한데, 만약 무기 바인더의 전체 무게에 대하여 0.1중량% 미만으로 첨가하게 되면 그 양이 너무 적어 강도의 증가효과가 미비하며, 반대로 그의 양을 0.5중량% 초과하여 첨가하게 되면 용해되지 않고 부유되거나 침전되는 알카리토금속 화합물이 발생되기 때문에 제조된 규산 바인더의 색도가 탁하며, 굽힘강도나 펠렛 타입강도가 측정부위마다 균일하지 못하다는 문제점이 발생하게 된다.The compound containing the alkaline earth metal added as described above is suitably added in an amount of 0.1 to 0.5% by weight based on the total weight of the prepared inorganic binder. If the amount is too small, the effect of increasing the strength is insignificant.On the contrary, when the amount is added in excess of 0.5% by weight, the alkali silicate compound which is not dissolved and suspended or precipitates is generated, so that the chromaticity of the manufactured silicate binder is turbid. There is a problem that the bending strength or pellet type strength is not uniform for each measurement site.
그 외에도 무기 바인더에 물성을 보강하기 위하여 규산소다와 염화수소 수용액의 반응 전에 무기물질을 첨가할 수 있으며, 이를 위해 소디움텅스티네이트(NaW04), 보락스(NaB407) 등을 용해시킨 후 사용할 수 있다. In addition, an inorganic substance may be added before the reaction between sodium silicate and aqueous hydrogen chloride solution to reinforce the physical properties of the inorganic binder. For this purpose, after dissolving sodium tungsten (NaW0 4 ) and borax (NaB 4 0 7 ), etc. Can be used.
이러한 방법을 제조된 무기 바인더는 접착제나 그라우팅제로 사용시 대기 중의 수분이나 물에 대하여 안정성을 가져 내수성이 좋고, 용도에 따라 강도를 조절할 수 있으며, 제조공정이 단순하고 생산설비가 간단하게 이루어지므로 제조비용을 낮출 수 있으며, 유해한 유기물을 용제로 사용하지 않고 물을 사용하기 때문에 환경친화적이라는 것이다.Inorganic binders prepared by this method have stability against moisture or water in the air when used as an adhesive or grouting agent, which has good water resistance, can adjust the strength according to the use, and the manufacturing process is simple and the production equipment is made simple. It is possible to lower the environment, and it is environmentally friendly because water is used instead of harmful organic substances as a solvent.
이하에서는 실시예를 통하여 본 발명을 좀 더 상세하게 설명하기는 하나, 하기의 실시예는 본 발명의 예시일 뿐, 본 발명이 하기의 실시예에 의하여 제한되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the following Examples are merely illustrative of the present invention, and the present invention is not limited by the following Examples.
<실시예 1><Example 1>
Na2O: 9%, SiO2: 29%의 조성을 갖는 액상 규산소다 1㎏을 100RPM으로 회전되는 반응기에 넣고, 물을 액상 규산소다에 대하여 30%가 되도록 첨가한 다음, 반응기 내의 온도를 40℃로 유지하고 3시간 동안 교반하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 하기와 같은 방법으로 강제건조에 따른 표면균열 및 내수성을 측정하여 그 측정값을 하기 표 1에 나타내었다.1 kg of liquid sodium silicate having a composition of 9% Na 2 O and 29% SiO 2 was added to a reactor rotated at 100 RPM, water was added to 30% with respect to liquid sodium silicate, and the temperature in the reactor was 40 ° C. It was maintained for 3 hours and stirred for 3 hours to prepare an inorganic binder, by measuring the surface crack and water resistance according to the forced drying in the manner described below for the inorganic binder prepared as shown in Table 1 below.
-표면균열-Surface Crack
carbon과 zeolite를 각각 1 : 1로 혼합한 혼합물에 무기 바인더를 전체 무게비에 대해 30%가 되도록 첨가하고 균일하게 혼합한 다음, 지름 2㎜/㎜의 구상으로 제립하고 dry oven(FO-600M)속에 삽입한 후, 강제적으로 열풍(90℃)을 가하여 순간적인 건조에 따른 표면의 균열정도를 하기와 같이 조사하여 각각의 무기 바인더에 대한 표면균열강도을 측정하였다.Inorganic binder was added to 30% of the total weight ratio and uniformly mixed with a mixture of carbon and zeolite 1: 1, and granulated in a sphere having a diameter of 2 mm / mm and placed in a dry oven (FO-600M). After insertion, hot air (90 ° C.) was forcibly applied, and the cracking degree of the surface due to instantaneous drying was examined as follows to measure the surface crack strength of each inorganic binder.
◎ ; 균열이 전혀 없음◎; No cracks at all
○ ; 균열이 미세하게 있음○; Fine cracks
△ ; 균열이 있음△; With cracks
× ; 균열상태가 심함×; Severe cracking
-내수성 실험-Water resistance test
펄라이트(perlite) 800g에 무기 바인더 240g을 첨가하고 균일하게 혼합한 다음, 가로 150㎜, 세로 80㎜, 두께 10㎜로 성형하고 130℃에서 60분간 건조하여 제조된 건조 시편을 3/4까지 물이 채워진 5ℓ용기에 24시간 동안 침전시킨 후 분해상 태를 조사하여 각각의 무기 바인더에 대한 내수성을 측정하였다.240 g of inorganic binder was added to 800 g of perlite and mixed uniformly. Then, the dried specimen prepared by molding 150 mm long, 80 mm long and 10 mm thick and drying at 130 ° C. for 60 minutes was filled with water. After precipitation for 24 hours in a filled 5 L container to determine the water resistance for each inorganic binder by examining the decomposition state.
◎ ; 물에 분해되지 않음◎; Not decompose in water
○; 물에 약간 분해됨 ○; Slightly degraded in water
△ ; 물에 분해됨△; Decomposed in water
×; 물에 완전히 분해됨 ×; Completely decomposed in water
<실시예 2><Example 2>
실시예 1과 동일한 방법으로 제조하되, 액상 규산소다에 포화농도의 염화수소 수용액(conc-HCl)을 액상 규산소다의 Na2O에 대하여 10%가 되도록 소량씩 첨가하고, 무기산 나트륨염의 결정이 생성될 때까지 약 1시간 동안 교반한 다음, 상기 결정체를 포함한 생성물에 물을 전체 무게에 대하여 30%가 되도록 첨가하고 다시 교반하여 결정체를 완전히 용해시켜 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 1과 동일한 방법으로 강제건조에 따른 표면균열 및 내수성을 측정하여 그 측정값을 하기 표 1에 나타내었다. Prepared in the same manner as in Example 1, but a small amount of saturated aqueous solution of hydrogen chloride (conc-HCl) is added to the liquid sodium silicate so as to be 10% of Na 2 O of the liquid sodium silicate, and crystals of the inorganic acid sodium salt may be formed. After stirring for about 1 hour, water was added to the product including the crystals to 30% of the total weight and stirred again to completely dissolve the crystals, thereby preparing an inorganic binder. Surface cracks and water resistance according to forced drying in the same manner as in Example 1 were measured and the measured values are shown in Table 1 below.
<실시예 3><Example 3>
실시예 2와 동일한 방법으로 제조하되, 액상 규산소다에 포화농도의 염화수소 수용액(conc-HCl)을 액상 규산소다의 Na2O에 대하여 20%가 되도록 소량씩 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 1과 동일한 방법으로 강제건조에 따른 표면균열 및 내수성을 측정하여 그 측정값을 하기 표 1에 나타내었다. Prepared in the same manner as in Example 2, but an inorganic binder was prepared by adding a small amount of saturated aqueous solution of hydrogen chloride (conc-HCl) to 20% with respect to Na 2 O of the liquid sodium silicate to the liquid sodium silicate to prepare an inorganic binder. In the same manner as in Example 1 for the prepared inorganic binder, the surface crack and water resistance according to the forced drying was measured and the measured values are shown in Table 1 below.
<실시예 4><Example 4>
실시예 2와 동일한 방법으로 제조하되, 액상 규산소다에 포화농도의 염화수소 수용액(conc-HCl)을 액상 규산소다의 Na2O에 대하여 25%가 되도록 소량씩 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 1과 동일한 방법으로 강제건조에 따른 표면균열 및 내수성을 측정하여 그 측정값을 하기 표 1에 나타내었다. Prepared in the same manner as in Example 2, but an inorganic binder was prepared by adding a small amount of saturated aqueous solution of hydrogen chloride (conc-HCl) to 25% of Na 2 O of the liquid sodium silicate to the liquid sodium silicate to prepare an inorganic binder. In the same manner as in Example 1 for the prepared inorganic binder, the surface crack and water resistance according to the forced drying was measured and the measured values are shown in Table 1 below.
<실시예 5><Example 5>
실시예 2와 동일한 방법으로 제조하되, 액상 규산소다에 포화농도의 염화수소 수용액(conc-HCl)을 액상 규산소다의 Na2O에 대하여 30%가 되도록 소량씩 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 1과 동일한 방법으로 강제건조에 따른 표면균열 및 내수성을 측정하여 그 측정값을 하기 표 1에 나타내었다. Prepared in the same manner as in Example 2, but an inorganic binder was prepared by adding a small amount of saturated aqueous solution of hydrogen chloride (conc-HCl) to 30% with respect to Na 2 O of the liquid sodium silicate. In the same manner as in Example 1 for the prepared inorganic binder, the surface crack and water resistance according to the forced drying was measured and the measured values are shown in Table 1 below.
<실시예 6><Example 6>
실시예 2와 동일한 방법으로 제조하되, 액상 규산소다에 포화농도의 염화수소 수용액(conc-HCl)을 액상 규산소다의 Na2O에 대하여 40%가 되도록 소량씩 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 1과 동일한 방법으로 강제건조에 따른 표면균열 및 내수성을 측정하여 그 측정값을 하기 표 1에 나타내었다. Prepared in the same manner as in Example 2, but an inorganic binder was prepared by adding a small amount of saturated aqueous solution of hydrogen chloride (conc-HCl) to 40% of Na 2 O of the liquid sodium silicate to the liquid sodium silicate to prepare an inorganic binder. In the same manner as in Example 1 for the prepared inorganic binder, the surface crack and water resistance according to the forced drying was measured and the measured values are shown in Table 1 below.
상기 표 1을 통하여 알 수 있듯이, 염화수소 수용액을 첨가하지 않은 실시예 1의 경우와 포화농도의 염화수소 수용액을 액상 규산소다의 산화나트륨에 대하여 10중량%가 되도록 첨가한 실시예 2의 경우에는 제조된 규산 바인더 내에 나트륨 이온이 다량 포함되어 있어 표면균열과 내수성에서 좋지 않음을 알 수 있었다.As can be seen from Table 1, prepared in the case of Example 1 is not added to the aqueous solution of hydrogen chloride and in the case of Example 2 added to the saturated aqueous solution of sodium chloride to 10% by weight of sodium hydroxide of the liquid sodium silicate prepared Sodium ions were contained in the silicic acid binder, which was not good in surface cracking and water resistance.
또한, 포화농도의 염화수소 수용액이 액상 규산소다의 산화나트륨에 대하여 20 내지 30중량%가 되도록 첨가한 실시예 3 내지 5의 경우에는 액상 규산소다에 포함된 나트륨 이온이 반응 후 염화나트륨염으로 침전되기 때문에 수분에 대하여 안정성을 가져 내수성이 좋고, 표면균열 측정에서도 좋게 평가되는 것을 알 수 있다.In addition, in the case of Examples 3 to 5 in which the saturated aqueous solution of hydrogen chloride was added in an amount of 20 to 30% by weight based on the sodium hydroxide in the liquid sodium silicate, sodium ions contained in the liquid sodium silicate precipitated as sodium chloride salt after the reaction. It has been found that it has stability against moisture, has good water resistance, and is well evaluated in surface crack measurement.
반면, 포화농도의 염화수소 수용액이 액상 규산소다의 산화나트륨에 대하여 40중량%를 첨가한 실시예 6의 경우에는 반응하여 생성된 규산물이 완전히 고형화되어 물에 용해되지 않아 바인더로서의 제조가 불가능하게 되는 것을 알 수 있었다. On the other hand, in the case of Example 6 in which the saturated aqueous hydrogen chloride solution added 40% by weight to the sodium hydroxide of the liquid sodium silicate, the silicic acid produced by the reaction was completely solidified and not dissolved in water, making it impossible to prepare as a binder. I could see that.
<실시예 7><Example 7>
실시예 5와 같이 제조된 무기 바인더에 대하여 하기와 같은 방법으로 굽힘강도 및 Pellet 강도를 측정하여 그 측정값을 하기 표 2에 나타내었다.For the inorganic binder prepared as in Example 5, the bending strength and pellet strength were measured by the following method, and the measured values are shown in Table 2 below.
-굽힘강도실험-Bending Strength Test
펄라이트(perlite) 800g에 무기 바인더 240g을 첨가하고 균일하게 혼합한 후, 가로 150㎜, 세로 80㎜, 두께 10㎜로 성형하고 130℃에서 건조하여 제조된 건조 시편을 UTM(모델:DTU-6207)장치를 이용하여 3등분점 재하법으로 평균변형속도를 약 5㎜/min으로 하여 하중을 가한 다음, 시험기가 나타내는 최대하중을 측정하고 하기 수학식 1을 이용하여 무기용 바인더에 대한 굽힘강도를 나타내었다.240 g of an inorganic binder was added to 800 g of perlite and uniformly mixed, followed by molding to 150 mm in width, 80 mm in thickness, and 10 mm in thickness, and drying at 130 ° C. to prepare a dry specimen of UTM (model: DTU-6207). Using the apparatus, load was applied at an average strain rate of about 5 mm / min using a three-point loading method, and then the maximum load indicated by the tester was measured, and the bending strength of the inorganic binder was expressed using Equation 1 below. It was.
{P : 최대하중(N), L : 시편의 길이(㎝), b : 시편의 나비(㎝), t : 시편의 두께(㎝)}{P: Maximum load (N), L: length of specimen (cm), b: butterfly of specimen (cm), t: thickness of specimen (cm)}
-Pellet type 강도실험-Pellet type strength test
carbon과 zeolite를 각각 1 : 1로 혼합한 혼합물에 무기 바인더를 전체 무게비에 대해 30%가 되도록 첨가하고 균일하게 혼합한 다음, 직경 2㎜, 길이 5㎜의 Pellet type으로 성형하고 120℃에서 건조한 후, IMADA(모델:DPS-20)장치를 이용하여 최대하중을 측정하고, 굽힘강도에 대한 수학식 1을 이용하여 각각 무기 바인더에 대한 Pellet type 강도를 측정하였다.Inorganic binder was added to 30% of the total weight ratio and uniformly mixed with a mixture of carbon and zeolite 1: 1, and then formed into pellet type of 2 mm diameter and 5 mm length and dried at 120 ° C. The maximum load was measured by using an IMADA (model: DPS-20) device, and the pellet type strength of the inorganic binder was measured using Equation 1 for bending strength.
<실시예 8><Example 8>
실시예 5와 동일한 방법으로 제조하되, 포화농도의 염화수소 수용액과 반응 후 생성된 규산물을 물에 용해시 염화마그네슘(MgCl2)을 전체 무게에 대하여 0.05%가 되도록 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 7과 동일한 방법으로 굽힘강도 및 Pellet 강도를 측정하여 그 측정값을 하기 표 2에 나타내었다.Prepared in the same manner as in Example 5, when dissolving the silicic acid produced after the reaction with a saturated aqueous solution of hydrogen chloride in water to add magnesium chloride (MgCl 2 ) to 0.05% of the total weight to prepare an inorganic binder, The bending strength and pellet strength of the inorganic binder thus prepared were measured in the same manner as in Example 7, and the measured values are shown in Table 2 below.
<실시예 9>Example 9
실시예 5와 동일한 방법으로 제조하되, 포화농도의 염화수소 수용액과 반응 후 생성된 규산물을 물에 용해시 염화마그네슘(MgCl2)을 전체 무게에 대하여 0.1%가 되도록 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 7과 동일한 방법으로 굽힘강도 및 Pellet 강도를 측정하여 그 측정값을 하기 표 2에 나타내었다.Prepared in the same manner as in Example 5, when dissolving the silicic acid produced after the reaction with a saturated aqueous solution of hydrogen chloride in water to add magnesium chloride (MgCl 2 ) to 0.1% of the total weight to prepare an inorganic binder, The bending strength and pellet strength of the inorganic binder thus prepared were measured in the same manner as in Example 7, and the measured values are shown in Table 2 below.
<실시예 10><Example 10>
실시예 5와 동일한 방법으로 제조하되, 포화농도의 염화수소 수용액과 반응 후 생성된 규산물을 물에 용해시 염화마그네슘(MgCl2)을 전체 무게에 대하여 0.5%가 되도록 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 7과 동일한 방법으로 굽힘강도 및 Pellet 강도를 측정하여 그 측정값을 하기 표 2에 나타내었다.Prepared in the same manner as in Example 5, when dissolving the silicic acid produced after the reaction with a saturated aqueous hydrogen chloride solution in water to prepare an inorganic binder by adding magnesium chloride (MgCl 2 ) to 0.5% of the total weight, The bending strength and pellet strength of the inorganic binder thus prepared were measured in the same manner as in Example 7, and the measured values are shown in Table 2 below.
<실시예 11><Example 11>
실시예 5와 동일한 방법으로 제조하되, 포화농도의 염화수소 수용액과 반응 후 생성된 규산물을 물에 용해시 염화마그네슘(MgCl2)을 전체 무게에 대하여 1.0%가 되도록 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 7과 동일한 방법으로 굽힘강도 및 Pellet 강도를 측정하여 그 측정값을 하기 표 2에 나타내었다.Prepared in the same manner as in Example 5, when dissolving the silicic acid produced after the reaction with a saturated aqueous solution of hydrogen chloride in water to add magnesium chloride (MgCl 2 ) to 1.0% of the total weight to prepare an inorganic binder, The bending strength and pellet strength of the inorganic binder thus prepared were measured in the same manner as in Example 7, and the measured values are shown in Table 2 below.
상기 표 2를 통하여 알 수 있듯이, 염화마그네슘이 첨가되지 않은 실시예 7과 비교하였을 경우, 염화마그네슘을 무기 바인더의 전체 무게에 대하여 0.05중량%가 되도록 첨가된 실시예 8에서는 굽힘강도와 펠렛타입 강도가 별로 차이가 없는 것을 알 수 있다.As can be seen from Table 2, when compared with Example 7 in which magnesium chloride is not added, in Example 8 in which magnesium chloride was added to 0.05% by weight based on the total weight of the inorganic binder, bending strength and pellet type strength It can be seen that there is not much difference.
반면, 염화마그네슘이 제조된 무기 바인더의 전체 무게에 대하여 0.1중량% 이상이 되도록 첨가한 실시예 9 내지 11의 경우에는 굽힘강도와 펠렛타입 강도가 월등하게 향상되는 것을 알 수 있으나, 다만 실시예 11의 경우에는 첨가되는 염화마그네슘이 모두 용해되지 않아 무기 바인더의 색도가 탁하며, 굽힘강도나 펠렛 타입강도가 측정부위에 따라 균일하지 못하다는 문제점이 발생하게 된다.On the other hand, in the case of Examples 9 to 11 added to the magnesium chloride to be at least 0.1% by weight relative to the total weight of the prepared inorganic binder, it can be seen that the bending strength and pellet type strength is significantly improved, but Example 11 In this case, all of the added magnesium chloride is not dissolved, so the color of the inorganic binder is turbid, and the bending strength or the pellet type strength is not uniform depending on the measurement site.
<실시예 12><Example 12>
Na2O: 5.5%, K2O: 2%, SiO2: 22.1%의 조성을 갖는 액상 규산소다 1㎏을 100RPM으로 회전되는 반응기에 넣고, 물 100g에 포화농도의 염화수소 수용액(conc-HCl) 15g을 천천히 적하시킨 다음, 반응기 내 온도를 40℃ 유지하면서 무기산 나트륨염의 결정이 생성될 때까지 약 1시간 동안 교반하였다. 1 kg of liquid sodium silicate having a composition of 5.5% Na 2 O, 2% K 2 O, and 22.1% SiO 2 was placed in a reactor rotated at 100 RPM, and 15 g of saturated aqueous hydrogen chloride (conc-HCl) was added to 100 g of water. Was slowly added dropwise, followed by stirring for about 1 hour until crystals of the sodium salt of the inorganic acid were formed while maintaining the temperature in the reactor at 40 ° C.
상기와 같이 결정체를 포함된 생성물에 물을 전체 무게에 대하여 30%가 되도록 첨가하고, 40℃에서 3시간 동안 교반하여 결정체를 완전히 용해시켜 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 하기와 같은 방법으로 압축강도와 산화나트륨의 용출량을 측정하여 하기 표 3에 나타내었다.Water was added to the product containing crystals as described above to 30% of the total weight, and stirred at 40 ° C. for 3 hours to completely dissolve the crystals to prepare an inorganic binder. Compression strength and elution amount of sodium oxide were measured in the same manner as shown in Table 3 below.
-압축강도실험-Compressive Strength Test
무기 바인더 70㎏과 물 130㎏이 혼합된 용액과 시멘트 120㎏과 물 80㎏이 혼합된 용액을 동시에 지름 5㎝, 높이 5㎝의 원형틀에 붓고 겔타임 이전에 혼합한 다음, 경화시켜 고화물을 형성시키고, 상기 고화물을 물에 담구고 1, 3, 7, 28일 후에 꺼내어 만능재료 시험기(UTM)로 압축강도를 측정하였다.70 kg of inorganic binder and 130 kg of water and 120 kg of cement and 80 kg of water were simultaneously poured into a circular frame of 5 cm in diameter and 5 cm in height, mixed before gel time, and cured. After the solids were immersed in water and taken out after 1, 3, 7, 28 days, the compressive strength was measured by a universal testing machine (UTM).
-산화나트륨의 용출량 측정-Measurement of elution amount of sodium oxide
KS M 1415에 따라, 압축강도실험을 위하여 제조되었던 고화물을 물에 담구고 1, 3, 7, 28일 후에 고화물이 담긴 물 2g을 채취하여 약 100㎖로 묽게 시킨 후, 0.1% 메틸오렌지 지시약 1방울을 가하여 1N염산으로 적정하고, 다시 1㎖를 과잉으로 가한 다음, 0.1N 수산화나트륨 용액으로 역적정하여 하기 수학식 2에 따라 산화나트륨의 용출량(%)을 계산하였다. In accordance with KS M 1415, the solids prepared for the compressive strength test were soaked in water, and after 1, 3, 7, 28 days, 2 g of the water containing the solids was collected and diluted to about 100 ml, followed by 0.1% methyl orange indicator. One drop was added, titrated with 1N hydrochloric acid, 1 ml was added excessively, and then back titrated with 0.1 N sodium hydroxide solution to calculate the elution amount (%) of sodium oxide according to the following equation (2).
{a : 적정에 소비된 1N 염산의 양(㎖), b : 역적정에 소비된 0.1N 수산화 나트륨의 양(㎖), S : 시료의 무게(g)}{a: amount of 1N hydrochloric acid consumed in titration (ml), b: amount of 0.1N sodium hydroxide consumed in reverse titration (ml), S: weight of sample (g)}
<실시예 13>Example 13
실시예 12와 동일한 방법으로 제조하되, 포화농도의 염화수소 수용액과 반응 후 생성된 규산물을 물에 용해시 황산마그네슘(MgSO4)을 전체 무게에 대하여 0.05%가 되도록 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 12와 동일한 방법으로 압축강도 및 산화나트륨의 용출량을 측정하여 하기 표 3에 나타내었다.Prepared in the same manner as in Example 12, when dissolving the silicic acid produced after the reaction with a saturated aqueous solution of hydrogen chloride in water to prepare an inorganic binder by adding magnesium sulfate (MgSO 4 ) to 0.05% of the total weight, Thus prepared inorganic binder was measured in the same manner as in Example 12 and the elution amount of sodium oxide was measured and shown in Table 3 below.
<실시예 14><Example 14>
실시예 12와 동일한 방법으로 제조하되, 포화농도의 염화수소 수용액과 반응 후 생성된 규산물을 물에 용해시 질산칼슘(Ca(NO3)2)을 전체 무게에 대하여 0.05%가 되도록 첨가하여 무기 바인더를 제조하고, 이와 같이 제조된 무기 바인더에 대하여 실시예 12와 동일한 방법으로 압축강도 및 산화나트륨의 용출량을 측정하여 하기 표 3에 나타내었다.Prepared in the same manner as in Example 12, but dissolving the siliceous product produced after the reaction with a saturated aqueous solution of hydrogen chloride in water to add calcium nitrate (Ca (NO 3 ) 2 ) to 0.05% of the total weight of the inorganic binder To prepare an inorganic binder prepared in this way, the compressive strength and the amount of elution of sodium oxide were measured in the same manner as in Example 12 and are shown in Table 3 below.
<비교예 1>Comparative Example 1
KS 3호 액상 규산소다(Na2O: 9%, SiO2: 28.5%함유)에 대하여 30%의 물을 첨가하고 교반시켜 제조된 무기 바인더에 대하여 실시에 45와 동일한 방법으로 압축강도와 산화나트륨의 용출량을 측정하여 하기 표 3에 나타내었다.Inorganic binder prepared by adding and stirring 30% water to KS No. 3 liquid sodium silicate (9% Na 2 O, containing 28.5% SiO 2 ) was stirred in the same manner as in Example 45 in terms of compressive strength and sodium oxide. The elution amount of was measured and shown in Table 3 below.
상기 표 3을 통하여 알 수 있듯이, 본 발명의 무기바인더를 그라우팅제로 사용한 실시예 12 내지 14의 경우 일반적인 규산소다 바인더를 그라우팅제로 사용한 비교예 1에 비하여 그 압축강도가 현저하게 증가됨을 알 수 있으며, 특히 7일이 지난 다음부터는 압축강도가 현저하게 차이가 남을 알 수 있다.As can be seen from Table 3, in the case of Examples 12 to 14 using the inorganic binder of the present invention as a grouting agent, it can be seen that the compressive strength is significantly increased compared to Comparative Example 1 using a general sodium silicate binder as a grouting agent, Especially after 7 days, it can be seen that the compressive strength is significantly different.
또한, 산화나트륨의 용출량의 경우에도 본 발명의 무기바인더를 그리우팅제로 사용한 실시예 12 내지 14가 비교예 1에 비하여 용출량이 훨씬 적게 나타나는 것을 알 수 있으며, 이는 내수성 측면에서 휠씬 개선된 것임을 알 수 있다.In addition, in the case of the elution amount of sodium oxide it can be seen that Examples 12 to 14 using the inorganic binder of the present invention as a grouting agent is much less than the comparative example 1, which is much improved in terms of water resistance. have.
상술한 바와 같이 본 발명의 액상 규산소다를 이용한 무기용 바인더의 제조방법은 액상 규산소다에 산용액으로서 포화농도의 염화수소 수용액을 일정배합량에 따라 첨가·교반하여 무기산 나트륨을 결정화하고 수용화시킴으로써, 대기 중의 수분이나 물에 대한 풀어짐 현상이 없는 내수성이 강한 무기 바인더의 제조가 가능하며, 제조장치가 간단하고 공정이 단순하여 전체적인 제조비용을 절감할 수 있고, 인체 및 환경에 유해한 유기용제를 사용하지 않아 환경친화적일 뿐만 아니라 알카리토금속을 함유하는 화합물을 일정량 첨가함으로써 굽힘강도나 강제건조에 따른 표면균열강도와 같은 물성을 향상시킬 수 있어 다양한 접착제와 그라우팅제로 유용한 효과를 가져오는 것이다.As described above, in the method for producing an inorganic binder using liquid sodium silicate of the present invention, an aqueous solution of saturated sodium chloride as an acid solution is added to the liquid sodium silicate and stirred according to a predetermined amount to crystallize and solubilize sodium inorganic acid. It is possible to manufacture inorganic binders with strong water resistance without releasing to water or water in the process, and the manufacturing apparatus is simple and the process is simple to reduce the overall manufacturing cost and does not use organic solvents that are harmful to human body and environment. In addition to being environmentally friendly, by adding a certain amount of a compound containing alkaline earth metal, it is possible to improve physical properties such as bending strength and surface crack strength due to forced drying, bringing useful effects with various adhesives and grouting agents.
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| KR102032840B1 (en) | 2017-09-25 | 2019-10-17 | 재단법인 한국탄소융합기술원 | Manufacturing method of inorganic heat insulating board using magnesium sulfate inorganic binder |
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