CN103483378A - Preparation method of organic phosphonateflame retardant - Google Patents
Preparation method of organic phosphonateflame retardant Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003063 flame retardant Substances 0.000 claims abstract description 52
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- MLCHBQKMVKNBOV-UHFFFAOYSA-N phenylphosphinic acid Chemical compound OP(=O)C1=CC=CC=C1 MLCHBQKMVKNBOV-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 6
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- XYFCBTPGUUZFHI-UHFFFAOYSA-N phosphine group Chemical group P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 14
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 6
- 239000000126 substance Substances 0.000 claims 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 36
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 abstract description 29
- 238000000034 method Methods 0.000 abstract description 23
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 3
- 239000013067 intermediate product Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- 235000019341 magnesium sulphate Nutrition 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001669 calcium Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IMDXZWRLUZPMDH-UHFFFAOYSA-N dichlorophenylphosphine Chemical compound ClP(Cl)C1=CC=CC=C1 IMDXZWRLUZPMDH-UHFFFAOYSA-N 0.000 description 1
- MLCHBQKMVKNBOV-UHFFFAOYSA-M dioxido(phenyl)phosphanium Chemical compound [O-]P(=O)C1=CC=CC=C1 MLCHBQKMVKNBOV-UHFFFAOYSA-M 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明涉及一种有机次膦酸盐阻燃剂的制备方法，合成步骤如下：在20～40℃的温度下，将苯基次膦酸加入到适量的水中，持续搅拌至完全溶解，加入金属盐或金属氢氧化物，逐渐升温至60～90℃，维持反应3～10小时；降温至室温，过滤，干燥即得有机次膦酸盐阻燃剂。本发明的一种有机次膦酸盐阻燃剂的制备方法，由简单易得的原料出发，不需要中间产物的分离，反应周期短，工艺简单易行，成本低，性价比高，得到的产品热稳定性好，具有良好的应用前景。
The invention relates to a preparation method of an organic phosphinate flame retardant. The synthesis steps are as follows: at a temperature of 20-40°C, add phenylphosphinic acid into an appropriate amount of water, keep stirring until completely dissolved, add metal Salt or metal hydroxide, the temperature is gradually raised to 60-90°C, and the reaction is maintained for 3-10 hours; the temperature is lowered to room temperature, filtered, and dried to obtain an organic phosphinate flame retardant. The preparation method of an organic phosphinate flame retardant of the present invention starts from simple and easy-to-obtain raw materials, does not require the separation of intermediate products, has a short reaction cycle, simple and easy process, low cost and high cost performance, and the obtained product Good thermal stability and good application prospects.
Description
技术领域technical field
本发明涉及一种有机次膦酸盐阻燃剂的制备方法。The invention relates to a preparation method of an organic phosphinate flame retardant.
背景技术Background technique
二十世纪80年代以来，阻燃剂已成为仅次于增塑剂的合成材料用量最大的助剂。随着经济的发展，人们的环保和安全意识有了很大提高，对生态环境和生命价值也更为关注。传统的卤系阻燃剂由于其阻燃效率高而被大量用于阻燃材料的生产，但由于卤系阻燃剂产品在燃烧时产生了大量的烟雾和有毒的腐蚀性气体，严重影响了火灾营救及人员疏散，导致二次灾难发生。因此，越来越多的国家开始禁止卤系阻燃产品的使用，而此时无卤阻燃剂由于具有低烟、低毒等环境友好型特点，逐渐得到广泛应用。使用高效、低烟、无毒或低毒的无卤阻燃剂将成为未来阻燃材料发展的必然趋势，近年来无机填充阻燃剂和膦系阻燃剂受到普遍关注。Since the 1980s, flame retardants have become the largest additives used in synthetic materials next to plasticizers. With the development of the economy, people's awareness of environmental protection and safety has greatly improved, and they are more concerned about the ecological environment and the value of life. Traditional halogenated flame retardants are widely used in the production of flame retardant materials due to their high flame retardant efficiency. Fire rescue and personnel evacuation led to secondary disasters. Therefore, more and more countries have begun to ban the use of halogen-based flame retardant products. At this time, halogen-free flame retardants are gradually being widely used due to their environmental friendliness such as low smoke and low toxicity. The use of high-efficiency, low-smoke, non-toxic or low-toxic halogen-free flame retardants will become an inevitable trend in the development of flame-retardant materials in the future. In recent years, inorganic-filled flame retardants and phosphine-based flame retardants have received widespread attention.
磷系阻燃剂由于阻燃效率高而在无卤阻燃领域备受重视。传统的磷系阻燃剂大多数具有挥发性，易水解等缺陷，因此开发大分子低挥发性、不易水解的磷系阻燃剂是今后开发的重点。有机次次膦酸盐因其良好的阻燃性能，使用时在性价比上有突出的优势，是卤系阻燃剂代用品中最有竞争力的品种之一。CN102174060A提出了苯基次次膦酸盐类阻燃剂的制备方法，采用苯基二氯化膦与金属盐反应，相比较本方法，反应速度慢，合成工艺耗时长，不利于大规模生产。Phosphorus-based flame retardants have attracted much attention in the field of halogen-free flame retardants due to their high flame retardant efficiency. Most of the traditional phosphorus-based flame retardants have defects such as volatility and easy hydrolysis. Therefore, the development of phosphorus-based flame retardants with low volatility and low hydrolysis of macromolecules is the focus of future development. Due to its good flame retardant properties, organic phosphinates have outstanding advantages in cost performance when used, and are one of the most competitive varieties of halogenated flame retardant substitutes. CN102174060A proposes a method for preparing phenylphosphinate flame retardants, which uses phenylphosphine dichloride to react with metal salts. Compared with this method, the reaction speed is slow, and the synthesis process takes a long time, which is not conducive to large-scale production.
发明内容Contents of the invention
本发明的目的是提供一种有机次膦酸盐阻燃剂的制备方法，采用不同合成工艺，制备工艺更加简单易行，有效降低人力及其他成本。The purpose of the present invention is to provide a method for preparing an organic phosphinate flame retardant, which adopts different synthesis processes, the preparation process is simpler, and the manpower and other costs are effectively reduced.
本发明的一种有机次膦酸盐阻燃剂的制备方法，合成步骤如下：在20～40℃的温度下，A kind of preparation method of organic phosphinate flame retardant of the present invention, synthetic steps are as follows: at the temperature of 20～40 ℃,
将苯基次膦酸加入到适量的水中，持续搅拌至完全溶解，加入金属盐或者金属氢氧化物，逐渐升温至60～90℃，维持反应3～10小时；降温至室温，过滤，干燥即得有机次膦酸盐阻燃剂。Add phenylphosphinic acid to an appropriate amount of water, keep stirring until completely dissolved, add metal salt or metal hydroxide, gradually raise the temperature to 60-90°C, and keep the reaction for 3-10 hours; cool down to room temperature, filter, and dry. Obtain organic phosphinate flame retardant.
作为优选的技术方案：As a preferred technical solution:
如上所述的一种有机次膦酸盐阻燃剂的制备方法，水的体积:苯基次膦酸的物质的量：金属盐或金属氢氧化物的物质的量=1L:1～2mol:1～5mol。A method for preparing an organic phosphinate flame retardant as described above, the volume of water: the amount of phenylphosphinic acid: the amount of metal salt or metal hydroxide = 1L: 1 ~ 2mol: 1～5mol.
如上所述的一种有机次膦酸盐阻燃剂的制备方法，所述金属盐或氢氧化物是氢氧化铝、氢氧化镁、氯化铝、氢氧化钙、氯化镁、氯化钙、硫酸铝、硫酸镁和硫酸锌中的至少一种。A method for preparing an organic phosphinate flame retardant as described above, the metal salt or hydroxide is aluminum hydroxide, magnesium hydroxide, aluminum chloride, calcium hydroxide, magnesium chloride, calcium chloride, sulfuric acid At least one of aluminum, magnesium sulfate and zinc sulfate.
如上所述的一种有机次膦酸盐阻燃剂的制备方法，所述有机次膦酸盐阻燃剂制成后粉碎至D90≤5um。A method for preparing an organic phosphinate flame retardant as described above, wherein the organic phosphinate flame retardant is pulverized to a D 90 ≤ 5um after being prepared.
有益效果：Beneficial effect:
本发明的一种有机次膦酸盐阻燃剂的制备方法，由简单易得的原料出发，不需要中间产物的分离，反应周期短，工艺简单易行，成本低，性价比高，得到的产品热稳定性好，具有良好的应用前景。The preparation method of an organic phosphinate flame retardant of the present invention starts from simple and easy-to-obtain raw materials, does not require the separation of intermediate products, has a short reaction cycle, simple and easy process, low cost and high cost performance, and the obtained product Good thermal stability and good application prospects.
附图说明Description of drawings
附图是本发明制备的次膦酸盐阻燃剂的TG图谱。Accompanying drawing is the TG spectrum of the phosphinate flame retardant prepared by the present invention.
具体实施方式Detailed ways
下面结合具体实施方式，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。The present invention will be further described below in combination with specific embodiments. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.
本发明的一种有机次膦酸盐阻燃剂的制备方法，合成步骤如下：在20～40℃的温度下，将苯基次膦酸加入到适量的水中，持续搅拌至完全溶解，加入金属盐或金属氢氧化物，维持反应3～10小时；降温至室温，过滤，干燥即得有机次膦酸盐阻燃剂，附图是本发明制备的次次膦酸盐阻燃剂的TG图谱。The preparation method of an organic phosphinate flame retardant of the present invention, the synthesis steps are as follows: at a temperature of 20-40°C, add phenylphosphinic acid to an appropriate amount of water, continue stirring until completely dissolved, add metal Salt or metal hydroxide, maintain the reaction for 3 to 10 hours; cool down to room temperature, filter, and dry to obtain the organic phosphinate flame retardant. The accompanying drawing is the TG spectrum of the phosphinate flame retardant prepared by the present invention .
如上所述的一种有机次膦酸盐阻燃剂的制备方法，水的体积：苯基次膦酸的物质的量：金属盐的物质的量=1L:1～2mol:1～5mol。A method for preparing an organic phosphinate flame retardant as described above, the volume of water: the amount of phenylphosphinic acid: the amount of metal salt = 1L: 1-2mol: 1-5mol.
如上所述的一种有机次膦酸盐阻燃剂的制备方法，所述金属盐或氢氧化物是氢氧化铝、氢氧化镁、氯化铝、氢氧化钙、氯化镁、氯化钙、硫酸铝、硫酸镁和硫酸锌中的至少一种。A method for preparing an organic phosphinate flame retardant as described above, the metal salt or hydroxide is aluminum hydroxide, magnesium hydroxide, aluminum chloride, calcium hydroxide, magnesium chloride, calcium chloride, sulfuric acid At least one of aluminum, magnesium sulfate and zinc sulfate.
如上所述的一种有机次膦酸盐阻燃剂的制备方法，所述有机次膦酸盐阻燃剂制成后粉碎至D90≤5um。A method for preparing an organic phosphinate flame retardant as described above, wherein the organic phosphinate flame retardant is pulverized to a D 90 ≤ 5um after being prepared.
实施例1Example 1
在带有搅拌的5L反应釜中，在50℃下，加入4L去离子水，加入2mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至70℃，待完全溶解后加入6mol氢氧化铝，维持反应3小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 5L reactor with stirring, at 50°C, add 4L of deionized water, add 2mol of phenylphosphinic acid, continue to stir, gradually increase the temperature to 70°C during the stirring process, and add 6mol of hydroxide after it is completely dissolved Aluminum, maintain the reaction for 3 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例2：Example 2:
在带有搅拌的2L反应釜中，在40℃下，加入1L去离子水，加入1mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至80℃，待完全溶解后加入2mol氢氧化镁，维持反应6小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 2L reaction kettle with stirring, at 40°C, add 1L of deionized water, add 1mol of phenylphosphinic acid, continue to stir, gradually increase the temperature to 80°C during the stirring process, and add 2mol of hydroxide after it is completely dissolved Magnesium, maintain the reaction for 6 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例3：Example 3:
在带有搅拌的20L反应釜中，在30℃下，加入15L去离子水，加入20mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至50℃，待完全溶解后加入70mol氯化铝，维持反应10小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 20L reactor with stirring, at 30°C, add 15L of deionized water, add 20mol of phenylphosphinic acid, continue to stir, gradually increase the temperature to 50°C during the stirring process, and add 70mol of chlorinated Aluminum, maintain the reaction for 10 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例4：Example 4:
在带有搅拌的500L反应釜中，在40℃下，加入200L去离子水，加入250mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至70℃，待完全溶解后加入550mol硫酸镁，维持反应4小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 500L reactor with stirring, at 40°C, add 200L of deionized water, add 250mol of phenylphosphinic acid, continue to stir, gradually heat up to 70°C during the stirring process, and add 550mol of magnesium sulfate after it is completely dissolved , maintain the reaction for 4 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例5：Example 5:
在带有搅拌的500L反应釜中，在50℃下，加入200L去离子水，加入200mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至90℃，待完全溶解后加入350mol氢氧化钙，维持反应10小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 500L reactor with stirring, at 50°C, add 200L deionized water, add 200mol phenylphosphinic acid, continue to stir, gradually increase the temperature to 90°C during the stirring process, and add 350mol hydroxide after it is completely dissolved Calcium, maintain the reaction for 10 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例6：Embodiment 6:
在带有搅拌的500L反应釜中，在30℃下，加入300L去离子水，加入300mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至80℃，待完全溶解后加入700mol氯化镁，维持反应8小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 500L reactor with stirring, at 30°C, add 300L of deionized water, add 300mol of phenylphosphinic acid, continue to stir, gradually heat up to 80°C during the stirring process, and add 700mol of magnesium chloride after it is completely dissolved. Maintain the reaction for 8 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例7：Embodiment 7:
在带有搅拌的500L反应釜中，在25℃下，加入400L去离子水，加入300mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至50℃，待完全溶解后加入650mol氯化钙，维持反应6小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 500L reactor with stirring, at 25°C, add 400L deionized water, add 300mol phenylphosphinic acid, keep stirring, gradually heat up to 50°C during the stirring process, and add 650mol chlorinated Calcium, maintain the reaction for 6 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例8：Embodiment 8:
在带有搅拌的200L反应釜中，在40℃下，加入100L去离子水，加入50mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至90℃，待完全溶解后加入200mol硫酸铝，维持反应8小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 200L reactor with stirring, at 40°C, add 100L of deionized water, add 50mol of phenylphosphinic acid, continue to stir, gradually heat up to 90°C during the stirring process, and add 200mol of aluminum sulfate after it is completely dissolved , maintain the reaction for 8 hours, then filter and dry to obtain an organic phosphinate flame retardant.
实施例9：Embodiment 9:
在带有搅拌的500L反应釜中，在30℃下，加入400L去离子水，加入100mol苯基次膦酸，持续搅拌，在搅拌过程中逐渐升温至70℃，待完全溶解后加入150mol硫酸锌，维持反应4小时，然后过滤，干燥，即得到一种有机次膦酸盐阻燃剂。In a 500L reactor with stirring, at 30°C, add 400L of deionized water, add 100mol of phenylphosphinic acid, continue to stir, gradually increase the temperature to 70°C during the stirring process, and add 150mol of zinc sulfate after it is completely dissolved , maintain the reaction for 4 hours, then filter and dry to obtain an organic phosphinate flame retardant.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5780534A (en) * | 1994-08-31 | 1998-07-14 | Ticona Gmbh | Flameproofed polyester molding composition |
| CN102174060A (en) * | 2011-01-25 | 2011-09-07 | 普塞呋（清远）磷化学有限公司 | Method for preparing phenyl hypophosphite flame retardant |
| CN102718798A (en) * | 2012-05-21 | 2012-10-10 | 金发科技股份有限公司 | Salts of dialkylphosphinic acid, preparation method and application |
-
2013
- 2013-09-05 CN CN201310401212.6A patent/CN103483378A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5780534A (en) * | 1994-08-31 | 1998-07-14 | Ticona Gmbh | Flameproofed polyester molding composition |
| CN102174060A (en) * | 2011-01-25 | 2011-09-07 | 普塞呋（清远）磷化学有限公司 | Method for preparing phenyl hypophosphite flame retardant |
| CN102718798A (en) * | 2012-05-21 | 2012-10-10 | 金发科技股份有限公司 | Salts of dialkylphosphinic acid, preparation method and application |
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| CN103980662A (en) * | 2014-04-01 | 2014-08-13 | 江汉大学 | Flame-retardant epoxy resin composition and preparation method thereof |
| CN103980662B (en) * | 2014-04-01 | 2016-08-31 | 江汉大学 | A kind of ethoxyline resin antiflaming compositions and preparation method thereof |
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