CN110819284A - Preparation method of silane-terminated sealant with excellent environmental protection and flame retardance - Google Patents
Preparation method of silane-terminated sealant with excellent environmental protection and flame retardance Download PDFInfo
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- CN110819284A CN110819284A CN201911123029.8A CN201911123029A CN110819284A CN 110819284 A CN110819284 A CN 110819284A CN 201911123029 A CN201911123029 A CN 201911123029A CN 110819284 A CN110819284 A CN 110819284A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to a preparation method of an environment-friendly silyl-terminated elastic sealant with excellent flame retardance, which comprises the following steps of: adding 15-25 parts of silyl-terminated polymer, 10-20 parts of plasticizer, 50-70 parts of filler, 0.5-5 parts of pigment, 1-2 parts of antioxidant, 1-2 parts of ultraviolet absorber and 1-2 parts of light stabilizer into a double-planet stirring kettle in sequence, adding 1-5 parts of water removing agent into the double-planet stirring kettle, adding 1-5 parts of tackifier into the stirring kettle, adding 0.5-2 parts of catalyst into the stirring kettle, mixing and packaging. The environmental protection fire retardant ammonium polyphosphate that adopts in this patent is a good performance's non-halogen fire retardant, adopts special technology to carry out chemical cladding to ammonium polyphosphate, makes it have splendid water-fast effect, stronger resistant mobility, good dispersibility, better heat stability, and flame retardant efficiency obviously strengthens.
Description
Technical Field
The invention relates to a preparation method of an environment-friendly silyl-terminated elastic sealant with excellent flame retardance, belonging to the field of adhesives.
Background
The elastic sealing gum with the silane end group can be divided into two categories of polyether elastic sealing gum with the silane end group and polyurethane elastic sealing gum with the silane end group. In recent years, due to the change of the organosilicon market, the price of raw materials rises and falls very little, and the silyl-terminated elastic sealant integrates the advantages of polyurethane sealant and organosilicon sealant, has better weather resistance and durability, good adhesion, paintability, environmental friendliness, low stain property and better construction performance, and more people aim at the silyl-terminated elastic sealant. The flame-retardant polypropylene composite material has excellent comprehensive performance and moderate price, is widely applied to a plurality of fields, and provides higher requirements for the flame retardance of the flame-retardant polypropylene composite material for customers.
Disclosure of Invention
The invention provides a preparation method of an environment-friendly silyl-terminated elastic sealant with excellent flame retardance, the flame retardance grade of the sealant prepared by the invention can reach V-0, the sealant has good adhesion on most base materials, and the requirements of flame retardance and reliability of products in the using process can be well met.
The preparation method of the silyl-terminated elastic sealant with environmental protection and excellent flame retardance comprises the following steps of: sequentially adding 15-25 parts of silyl-terminated polymer, 10-20 parts of plasticizer, 50-70 parts of filler, 0.5-5 parts of pigment, 1-2 parts of antioxidant, 1-2 parts of ultraviolet absorber and 1-2 parts of light stabilizer into a double-planet stirring kettle, stirring and dispersing at 100-110 ℃ and carrying out vacuum dehydration for 2 hours, wherein the vacuum degree is not less than-0.098 MPa, cooling to below 45 ℃, adding 1-5 parts of water removing agent into the double-planet stirring kettle, mixing for 30 minutes in a vacuum state, adding 1-5 parts of tackifier into the stirring kettle, mixing for 10 minutes in a vacuum state, finally adding 0.5-2 parts of catalyst into the stirring kettle, mixing for 10 minutes in a vacuum state, wherein the vacuum degree is not less than-0.098 MPa, and N is used as a stabilizer2Sealing and packaging.
The ammonium polyphosphate used as the environment-friendly flame retardant in the patent is a non-halogen flame retardant with excellent performance, is nontoxic and tasteless, and has the excellent characteristics of high-efficiency flame retardance, environmental friendliness, small addition amount, small mechanical property influence and the like. But the self-adhesive has the defects of poor compatibility with the polymer and poor dialysis resistance, once the surface of the polymer is separated out, the polymer is easy to absorb moisture, dissolve in water and hydrolyze in a humid environment, the weather resistance and the electrical property of the polymer are influenced, and the application range of the polymer is limited. The method selects proper materials, adopts a special process to carry out chemical coating on ammonium polyphosphate, and has the advantages of excellent water-resistant effect, strong migration resistance, good dispersibility, good thermal stability and obviously enhanced flame-retardant effect. On the basis of the technical scheme, the invention can be further improved as follows.
Further, the silane-terminated polymer has a polymer of the following structural formula (1) or structural formula (2):
structural formula (1)
Structural formula (2)
R1= one of methyl, ethyl, methoxy, ethoxy,
R2either methoxy group or ethoxy group,
R3=-CH2-、-(CH2)3-。
further, the plasticizer is one or a mixture of several of diisononyl phthalate (DINP), diisodecyl phthalate (DIDP), phenyl alkylsulfonate, and SAT015 of KANEKA, Japan.
Further, the filler is a mixture of several of nano active calcium carbonate, aluminum hydroxide, magnesium hydroxide and an environment-friendly flame retardant ammonium polyphosphate, and the amount of the filler is 0-20 parts, 0-40 parts, 0-35 parts and 0-20 parts by mass respectively.
Ammonium polyphosphate pretreatment: adding ammonium polyphosphate into a stirring kettle, slowly dropwise adding an aqueous solution with the concentration of 2.0-5.0wt% of a coupling agent KBM-303 [2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane ] while stirring, stirring for 2 hours at room temperature, then heating to 120 plus 130 ℃, vacuumizing and continuously stirring for 5 hours, then closing heating, maintaining pressure, cooling to room temperature, discharging, filtering, and drying for later use.
Further, the pigment is one of titanium dioxide and carbon black.
Further, the antioxidant is one of an antioxidant 1010 and an antioxidant 1076.
Further, the light stabilizer is bis (2,2, 6, 6-tetramethyl-4-piperidyl) sebacate, namely a light stabilizer 770.
Further, the ultraviolet absorber is 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole, namely the ultraviolet absorber UV-326.
Further, the water removing agent is vinyl trimethoxy silane.
Further, the tackifier is one or a mixture of N- β -aminoethyl-gamma-aminopropyltrimethoxysilane, aminopropyltrimethoxysilane and aminopropyltriethoxysilane.
Further, the catalyst is one or a mixture of more of U-220H, U-303 and stannous octoate formed by chemical reaction in the east China.
The invention has the beneficial effects that: the silyl-terminated elastic sealant with excellent flame retardance provided by the invention is packaged by single components, is easy to glue, has low density, does not emit toxic gas after being cured, and has higher adhesive force to various substrates.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Ammonium polyphosphate pretreatment: adding ammonium polyphosphate into a stirring kettle, slowly dropwise adding an aqueous solution with the concentration of 2.0-5.0wt% of a coupling agent KBM-303 [2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane ] while stirring, wherein the amount of the aqueous solution is 15-25% of the total amount of the ammonium polyphosphate, stirring for 2 hours at room temperature, then heating to 120 ℃ and 130 ℃, vacuumizing and continuously stirring for 5 hours, then closing heating, maintaining pressure, cooling to room temperature, discharging, filtering and drying for later use, wherein the ammonium polyphosphate used in the following embodiments is treated.
Example 1
15 parts of a silane-terminated polymer of the formula
10 parts of diisononyl phthalate, 10 parts of nano active calcium carbonate, 25 parts of aluminum hydroxide, 15 parts of environment-friendly flame retardant ammonium polyphosphate, 0.5 part of titanium dioxide, 1 part of antioxidant 1010, 1 part of light stabilizer 770 and 1 part of ultraviolet absorbent UV-326 are sequentially added into a double-planetary stirring kettle, stirred, dispersed and vacuum-dehydrated for 2 hours at the temperature of 100-110 ℃, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to the temperature below 45 ℃,1 part of vinyl trimethoxy silane is added into the double-planetary stirring kettle and mixed for 30 minutes under the vacuum state, then 1.0 part of N- β -aminoethyl-gamma-aminopropyl trimethoxy silane is added into the double-planetary stirring kettle and mixed for 10 minutes under the vacuum state, and finally 0.5 part of U-220H is added into the stirring kettle and mixed for 10 minutes under the vacuum state, the vacuum degree is not less than-0.098 MPa, and the N is not less than2Sealing and packaging.
Example 2
25 parts of a silane-terminated polymer of the formula
20 parts of diisodecyl phthalate, 20 parts of nano active calcium carbonate, 30 parts of aluminum hydroxide, 20 parts of environment-friendly flame retardant ammonium polyphosphate, 5 parts of titanium dioxide, 2 parts of antioxidant 1076, 2 parts of light stabilizer 770 and 2 parts of ultraviolet absorbent UV-326 are sequentially added into a double-planet stirring kettle, stirred, dispersed and vacuum-dehydrated for 2 hours at the temperature of 100-110 ℃, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to the temperature of below 45 ℃, 5 parts of vinyl trimethoxy silane is added into the double-planet stirring kettle, mixed for 30 minutes in the vacuum state, then 5 parts of aminopropyl triethoxy silane is added into the double-planet stirring kettle, mixed for 10 minutes in the vacuum state, finally 1 part of U-303 and 1 part of stannous octoate are added into the stirring kettle, mixed for 10 minutes in the vacuum state, the vacuum degree is not less than-0.098 MPa, N is added into the double-planet stirring2Sealing and packaging.
Example 3
20 parts of silane-terminated polymer with the structural formula
10 parts of SAT015, 5 parts of diisononyl phthalate, 5 parts of nano active calcium carbonate, 35 parts of magnesium hydroxide, 15 parts of environment-friendly flame retardant ammonium polyphosphate, 2.5 parts of carbon black, 1.5 parts of antioxidant 1010, 1.5 parts of light stabilizer 770 and 1.5 parts of ultraviolet absorbent UV-326 are sequentially added into a double-planet stirring kettle, stirred, dispersed and vacuum-dehydrated for 2 hours at the temperature of 100-110 ℃, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to below 45 ℃, 3 parts of vinyl trimethoxy silane is added into the double-planet stirring kettle and mixed for 30 minutes under the vacuum state, then 3 parts of aminopropyl trimethoxy silane is added into the double-planet stirring kettle and mixed for 10 minutes under the vacuum state, finally 1 part of stannous octoate is added into the stirring kettle and mixed for 10 minutes under the vacuum state, the vacuum degree is not less than-0.098 MPa, N is added into the double-planet stirring kettle2Sealing and packaging.
Example 4
20 parts of silane-terminated polymer with the structural formula
15 parts of phenyl alkyl sulfonate, 10 parts of nano active calcium carbonate, 40 parts of aluminum hydroxide, 5 parts of environment-friendly flame retardant ammonium polyphosphate, 2 parts of carbon black, 1.5 parts of antioxidant 1076, 2 parts of light stabilizer 770 and 2 parts of ultraviolet absorbent UV-326 are sequentially added into a double-planetary stirring kettle, stirred, dispersed and vacuum-dehydrated for 2 hours at the temperature of 100-110 ℃, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to the temperature of below 45 ℃, 2.5 parts of vinyl trimethoxy silane is added into the double-planetary stirring kettle, mixed for 30 minutes under the vacuum state, then 1.5 parts of N- β -aminoethyl-gamma-aminopropyl trimethoxy silane and 1 part of aminopropyl triethoxy silane are added into the double-planetary stirring kettle, mixed for 10 minutes under the vacuum state, finally 1.5 parts of U-220H is added into the stirring kettle, mixed for 10 minutes under the vacuum state, and the vacuum degree is not less than-0.098 MPa , N2Sealing and packaging.
The performance comparison tests of the examples 1 to 4 and the general-purpose silane-terminated polyether sealant are carried out, the flame retardant performance data are obtained by testing after the sealant is cured for 7 days under the conditions of 23 +/-2 ℃ and 50 +/-5% of relative humidity, and the specific test results are shown in the following table 1.
Test examples
The performance of a silane-terminated sealant of the present invention having excellent media resistance was tested by the following test.
Test example 1
The vertical burning test was carried out according to GB/T5169.16-2008.
The general purpose silyl terminated elastomeric sealants were compared to examples 1, 2, 3,4 for performance testing,
| test items | General purpose Model (III) | Examples of the invention 1 | Examples of the invention 2 | Examples of the invention 3 | Examples of the invention 4 |
| Afterflame time, s, of individual test specimens | ＞30 | 8 | 2 | 2 | 6 |
| For any pretreatment, total afterflame time, s | ＞250 | 45 | 30 | 31 | 40 |
| After the second application of flame, the afterflame time of the individual test specimens was increased Burning time of upper part, s | ＞60 | 28 | 19 | 20 | 25 |
| Whether or not after flame and/or after burning has spread to the holding jig | Is that | Whether or not | Whether or not | Whether or not | Whether or not |
| Whether the burning particles or drops ignite the cotton pad | Is that | Whether or not | Whether or not | Whether or not | Whether or not |
| UL-94 | V-1 | V-0 | V-0 | V-0 | V-0 |
The test results in the table show that the silyl-terminated elastic sealant with excellent flame retardance has good flame retardance and can reach the V-0 standard, and the flame retardance effect is more prominent by compounding the inorganic flame retardant (aluminum hydroxide and magnesium hydroxide) and the environment-friendly flame retardant ammonium polyphosphate, and is obviously superior to the domestic common silyl-terminated elastic sealant products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. The preparation method of the silane-terminated sealant with environmental protection and excellent flame retardance is characterized by comprising the following steps of: sequentially adding 15-25 parts of silyl-terminated polymer, 10-20 parts of plasticizer, 50-70 parts of filler, 0.5-5 parts of pigment, 1-2 parts of antioxidant, 1-2 parts of ultraviolet absorber and 1-2 parts of light stabilizer into a double-planet stirring kettle, stirring and dispersing at 100-110 ℃ and carrying out vacuum dehydration for 2 hours, wherein the vacuum degree is not less than-0.098 MPa, cooling to below 45 ℃, adding 1-5 parts of water removing agent into the double-planet stirring kettle, mixing for 30 minutes in a vacuum state, adding 1-5 parts of tackifier into the stirring kettle, mixing for 10 minutes in a vacuum state, finally adding 0.5-2 parts of catalyst into the stirring kettle, mixing for 10 minutes in a vacuum state, wherein the vacuum degree is not less than-0.098 MPa, and N is used as a stabilizer2Sealing and packaging;
the filler is a mixture of several of nano active calcium carbonate, aluminum hydroxide, magnesium hydroxide and an environment-friendly flame retardant ammonium polyphosphate, and the using amounts of the filler are 0-20 parts, 0-40 parts, 0-35 parts and 0-20 parts by mass respectively;
the ammonium polyphosphate pretreatment comprises the following steps: adding ammonium polyphosphate into a stirring kettle, slowly dropwise adding an aqueous solution with the concentration of 2.0-5.0wt% of a coupling agent KBM-303 [2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane ] while stirring, stirring for 2 hours at room temperature, then heating to 120 plus 130 ℃, vacuumizing and continuously stirring for 5 hours, then closing heating, maintaining pressure, cooling to room temperature, discharging, filtering, and drying for later use.
2. The method of claim 1 wherein the silane-terminated polymer is a polymer of the following formula (1) or formula (2):
structural formula (1)
Structural formula (2)
R1= one of methyl, ethyl, methoxy, ethoxy,
R2either methoxy group or ethoxy group,
R3=-CH2-、-(CH2)3-。
3. the method of preparing a silane-terminated sealant according to claim 1 wherein the plasticizer is one or a mixture of diisononyl phthalate, diisodecyl phthalate, phenyl alkylsulfonate, SAT015 of KANEKA, japan; the antioxidant is one of an antioxidant 1010 and an antioxidant 1076; the light stabilizer is bis (2,2, 6, 6-tetramethyl-4-piperidyl) sebacate; the ultraviolet light absorber is 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole; the water removing agent is vinyl trimethoxy silane.
4. The preparation method of the silane-terminated sealant according to claim 1, wherein the tackifier is one or a mixture of N- β -aminoethyl-gamma-aminopropyltrimethoxysilane, aminopropyltrimethoxysilane and aminopropyltriethoxysilane, and the catalyst is one or a mixture of U-220H, U-303 and stannous octoate which are formed by Nidong.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113105860A (en) * | 2021-03-19 | 2021-07-13 | 上海康达化工新材料集团股份有限公司 | Ultrafast-curing flame-retardant bi-component epoxy modified silyl-terminated polymer adhesive, and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113105860A (en) * | 2021-03-19 | 2021-07-13 | 上海康达化工新材料集团股份有限公司 | Ultrafast-curing flame-retardant bi-component epoxy modified silyl-terminated polymer adhesive, and preparation method and application thereof |
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