CN114133567B - Preparation method of polysiloxane cross-linking agent - Google Patents
Preparation method of polysiloxane cross-linking agent Download PDFInfo
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- CN114133567B CN114133567B CN202111064856.1A CN202111064856A CN114133567B CN 114133567 B CN114133567 B CN 114133567B CN 202111064856 A CN202111064856 A CN 202111064856A CN 114133567 B CN114133567 B CN 114133567B
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 48
- -1 polysiloxane Polymers 0.000 title claims abstract description 47
- 239000003431 cross linking reagent Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 126
- 238000001816 cooling Methods 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 23
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004806 packaging method and process Methods 0.000 claims abstract description 20
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229920002545 silicone oil Polymers 0.000 claims abstract description 12
- 230000035484 reaction time Effects 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims description 47
- 229920005989 resin Polymers 0.000 claims description 47
- 230000002378 acidificating effect Effects 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 21
- 239000011148 porous material Substances 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000012508 resin bead Substances 0.000 claims description 5
- 125000002091 cationic group Chemical group 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 40
- 230000000052 comparative effect Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- 238000007789 sealing Methods 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 7
- 150000001768 cations Chemical class 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000006459 hydrosilylation reaction Methods 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of a polysiloxane cross-linking agent, belonging to the technical field of cross-linking agent preparation. The preparation method of the polysiloxane crosslinking agent comprises the following steps: (1) feeding: the composition comprises the following raw materials in parts by weight: 1-2 parts of hexamethyldisiloxane and 2-30 parts of high-hydrogen silicone oil; 20-120 parts of siloxane mixed ring body; (2) telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, the reaction temperature is 80-90 ℃, and the reaction time is 4-8 hours; and (3) removing low molecules: conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules; and (4) cooling and packaging: and cooling and packaging the polysiloxane cross-linking agent product. The preparation method of the polysiloxane crosslinking agent has the advantages of skillful reaction kettle structure arrangement, high catalytic performance, high production efficiency, safety and environmental protection.
Description
Technical Field
The invention relates to the technical field of cross-linking agent preparation, in particular to a preparation method of a polysiloxane cross-linking agent.
Background
Polysiloxane cross-linking agent mainly refers to side hydrogen polysiloxane used for hydrosilylation, which is generally prepared by dimethyl cyclosiloxane (D4 or DMC) with low molar mass, high hydrogen silicone oil and hexamethyldisiloxane by a kettle type reaction in industry. The common catalyst system is concentrated sulfuric acid, the process has the disadvantages of high material danger, complex neutralization process, low product yield, high byproduct treatment difficulty and more hidden dangers in the aspects of safety and environmental protection. In the resin catalysis process which is started in recent years, the produced polysiloxane product is tasteless and has better quality, but the fixed bed process can only prepare the product with the viscosity of less than 50 mPa.s, and the kettle type reaction can only produce the product with low viscosity because the filtration is not easy to operate, so the application field is greatly limited. According to the conventional process for preparing the silicone oil by using the reaction kettle, the acidic resin is directly mixed with the siloxane raw material in the reaction kettle for reaction, and after the reaction is finished, a settling or filtering mode is adopted for solid-liquid phase separation.
Disclosure of Invention
The invention aims to solve the technical problems of insufficient safety and environmental protection of the catalyst, low yield, high treatment difficulty, low yield of the generated product and low viscosity in the prior art, thereby providing the preparation method of the polysiloxane crosslinking agent.
The invention solves the problems and adopts the technical scheme that:
a method for preparing a polysiloxane cross-linking agent; the method comprises the following steps:
(1) Feeding: the feed comprises the following raw materials in parts by weight: 1-2 parts of hexamethyldisiloxane and 2-30 parts of high-hydrogen silicone oil; 20-120 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 80-90 ℃, and the reaction time is 4-8 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the polysiloxane cross-linking agent product with the low molecular weight removed, and packaging the obtained product.
Compared with the prior art, the invention adopting the technical scheme has the prominent characteristics that:
the invention provides a preparation method of a polysiloxane cross-linking agent, wherein acidic resin balls are fixed in an inner jacket and a cavity baffle of a reaction kettle, polysiloxane continuously enters and exits from pores of the inner jacket and the cavity baffle, and a polymerization equilibrium reaction is carried out in an acidic resin ball catalytic system. Polysiloxane is discharged after the reaction is finished, the solid phase and the liquid phase are automatically separated, the filtering step is avoided, the reaction kettle is skillfully arranged, the catalyst is high in performance, the safety and environmental protection performance are high, the production efficiency is high, the product yield is high, and the produced polysiloxane cross-linking agent is controllable in viscosity and good in cross-linking performance.
Preferably, the invention further comprises:
the end sealing agent in the step (1) is hexamethyldisiloxane.
In the step (1), before the siloxane mixed ring body is added into the reaction kettle, water needs to be removed.
And (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
The acidic resin balls in the step (2) are cationic acidic resin catalysts, the particle size of the acidic resin balls is 500-1000 mu m, and the pore diameter of the pores is 300 mu m.
The filling volume of the acidic resin balls in the step (2) is 5-15% of the total volume of the reaction kettle.
The low molecular weight removing device in the step (3) is a thin film evaporator or a distillation tower.
The vacuum degree of the low-molecular-weight-removing equipment in the step (3) is-0.099 MPa &0.09MPa below zero, and the temperature of low molecular weight removing equipment is 140-150 DEG C 。
And (4) cooling in the step (4) to remove the low molecular weight polysiloxane cross-linking agent product and cooling to room temperature.
Detailed Description
The invention will be further illustrated by the following examples, which are intended only for a better understanding of the present invention and therefore do not limit the scope of the invention.
The raw materials in the examples are conventional raw materials and are all purchased from the market.
Example 1
A method for preparing a polysiloxane crosslinking agent; the method comprises the following steps:
(1) Feeding: the composition comprises the following raw materials in parts by weight: 1 part of hexamethyldisiloxane and 2 parts of high hydrogen-containing silicone oil; 20 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 80 ℃, and the reaction time is 8 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the polysiloxane cross-linking agent product with the low molecular weight removed to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the siloxane mixed ring body must be dewatered before being added into the reaction kettle.
And (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
The acid resin ball in the step (2) is a cation acid resin catalyst, the particle size of the acid resin ball is 500-1000 μm, and the pore diameter of the pore is 300 μm.
The filling volume of the acidic resin balls in the step (2) is 5-15% of the total volume of the reaction kettle.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
The vacuum degree of the low molecular weight removing equipment in the step (3) is-0.099 MPa to-0.09 MPa, and the temperature of the low molecular weight removing equipment is 140-150 DEG C 。
And (5) cooling in the step (4) to remove the low molecular polysiloxane cross-linking agent product and cooling to room temperature.
Example 2
A method for preparing a polysiloxane crosslinking agent; the method comprises the following steps:
(1) Feeding: the composition comprises the following raw materials in parts by weight: 1 part of hexamethyldisiloxane and 2 parts of high hydrogen-containing silicone oil; 40 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 90 ℃, and the reaction time is 6 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the polysiloxane cross-linking agent product with the low molecular weight removed to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the siloxane mixed ring body must be dewatered before being added into the reaction kettle.
And (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
The acidic resin balls in the step (2) are cationic acidic resin catalysts, the particle size of the acidic resin balls is 500-1000 mu m, and the pore diameter of the pores is 300 mu m.
The filling volume of the acidic resin balls in the step (2) is 5-15% of the total volume of the reaction kettle.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
The vacuum degree of the low molecular removal equipment in the step (3) is-0.099 MPa to-0.09 MPa, the temperature of the low molecular removal equipment is 140-150 DEG C 。
And (5) cooling in the step (4) to remove the low molecular polysiloxane cross-linking agent product and cooling to room temperature.
Example 3
A method for preparing a polysiloxane crosslinking agent; the method comprises the following steps:
(1) Feeding: the composition comprises the following raw materials in parts by weight: 1 part of hexamethyldisiloxane and 5 parts of high hydrogen-containing silicone oil; 70 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 90 ℃, and the reaction time is 4 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the polysiloxane cross-linking agent product with the low molecular weight removed to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the siloxane mixed ring body must be dewatered before being added into the reaction kettle.
And (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
The acid resin ball in the step (2) is a cation acid resin catalyst, the particle size of the acid resin ball is 500-1000 μm, and the pore diameter of the pore is 300 μm.
The filling volume of the acidic resin balls in the step (2) is 5-15% of the total volume of the reaction kettle.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
The vacuum degree of the low molecular weight removing equipment in the step (3) is-0.099 MPa to-0.09 MPa, and the temperature of the low molecular weight removing equipment is 140-150 DEG C 。
And (4) cooling the product of the polysiloxane crosslinking agent with low molecular weight removed to room temperature.
Example 4
A method for preparing a polysiloxane crosslinking agent; the method comprises the following steps:
(1) Feeding: the feed comprises the following raw materials in parts by weight: 1 part of hexamethyldisiloxane and 5 parts of high hydrogen-containing silicone oil; 70 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 90 ℃, and the reaction time is 4 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the low molecular weight polysiloxane cross-linking agent removed product to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the water must be removed before the siloxane mixed ring is added to the reaction vessel.
And (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
The acid resin ball in the step (2) is a cation acid resin catalyst, the particle size of the acid resin ball is 500-1000 μm, and the pore diameter of the pore is 300 μm.
The filling volume of the acidic resin balls in the step (2) is 5-15% of the total volume of the reaction kettle.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
Equipment for removing low molecular weight in step (3)The vacuum degree is-0.099 MPa to-0.09 MPa, the temperature of the low molecular weight removing equipment is 140-150 DEG C 。
And (5) cooling in the step (4) to remove the low molecular polysiloxane cross-linking agent product and cooling to room temperature.
Example 5
A method for preparing a polysiloxane crosslinking agent; the method comprises the following steps:
(1) Feeding: the feed comprises the following raw materials in parts by weight: 2 parts of hexamethyldisiloxane and 20 parts of high hydrogen-containing silicone oil; 120 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 85 ℃, and the reaction time is 5 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the polysiloxane cross-linking agent product with the low molecular weight removed to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the siloxane mixed ring body must be dewatered before being added into the reaction kettle.
And (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
The acid resin ball in the step (2) is a cation acid resin catalyst, the particle size of the acid resin ball is 500-1000 μm, and the pore diameter of the pore is 300 μm.
The filling volume of the acidic resin balls in the step (2) is 5-15% of the total volume of the reaction kettle.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
The vacuum degree of the low molecular removal equipment in the step (3) is-0.099 MPa to-0.09 MPa, the temperature of the low molecular removal equipment is 140-150 DEG C 。
And (4) cooling the product of the polysiloxane crosslinking agent with low molecular weight removed to room temperature.
And (3) measuring the appearance, yield, viscosity, volatile content and acid value of the product to obtain the final product index shown in the table 1:
table 1: EXAMPLES polysiloxane crosslinker product specifications
Comparative example 1
Comparative example 1 the product was prepared using the following procedure:
(1) Feeding: the composition comprises the following raw materials in parts by weight: 2 parts of hexamethyldisiloxane and 20 parts of high hydrogen-containing silicone oil; 120 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, the reaction kettle adopts a common reaction kettle, the catalyst in the reaction kettle is concentrated sulfuric acid, the reaction temperature in the reaction kettle is 45 ℃, and the reaction time is 5 hours; adding sodium carbonate to neutralize the acid oil, and filtering after the neutralization is finished;
(3) Removing low molecules: conveying the filtered material to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the polysiloxane cross-linking agent product with the low molecular weight removed to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the siloxane mixed ring body must be dewatered before being added into the reaction kettle.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
The vacuum degree of the low molecular removal equipment in the step (3) is-0.099 MPa to-0.09 MPa, the temperature of the low molecular removal equipment is 140-150 DEG C 。
And (4) cooling the product of the polysiloxane crosslinking agent with low molecular weight removed to room temperature.
Comparative example 1 the feeding ratio and reaction process of example 5 were repeated, but concentrated sulfuric acid was used as the catalyst, the filtration process was slow, and the filtration was completed by replacing the filter paper several times. The product was observed and found to be cloudy in appearance despite filtration, with fine salts difficult to filter clean. The reaction activity of the product is tested by the addition reaction, and the hydrosilylation reaction is found to be incomplete and the system is turbid.
Comparative example 2
Comparative example 2 the product was prepared using the following procedure:
(1) Feeding: the composition comprises the following raw materials in parts by weight: 2 parts of hexamethyldisiloxane and 20 parts of high hydrogen-containing silicone oil; 120 parts of siloxane mixed ring body;
(2) Telomerization: carrying out equilibrium reaction on the raw materials through a fixed bed, wherein an acidic resin ball catalyst is filled in the fixed bed, the reaction temperature of the fixed bed is 85 ℃, and the reaction time is 5 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: and (3) cooling the low molecular weight polysiloxane cross-linking agent removed product to room temperature, and packaging the obtained product.
Wherein: the end sealing agent in the step (1) is hexamethyldisiloxane.
In step (1), the siloxane mixture ring must be dewatered before it is introduced into the fixed bed.
The acidic resin balls in the step (2) are cationic acidic resin catalysts, and the particle size of the acidic resin balls is 500-1000 microns.
The low molecular weight removing device in the step (3) is a film evaporator or a distillation tower.
The vacuum degree of the low molecular removal equipment in the step (3) is-0.099 MPa to-0.09 MPa, the temperature of the low molecular removal equipment is 140-150 DEG C 。
And (4) cooling the product of the polysiloxane crosslinking agent with low molecular weight removed to room temperature.
Comparative example 2 the feeding proportion and the reaction process of example 5 were repeated, the catalyst still used acidic resin beads, but the reaction equipment used fixed bed, and the reaction product could not be obtained due to the very slow flow rate of the material with high viscosity during the reaction process.
Finally, the cross-linking performance characterization of the cross-linking agents is carried out on the products of examples 1-5 and comparative examples, and the finally obtained cross-linking performance results are characterized as shown in table 2:
table 2: crosslinking effect of the product
| Preparation of the product | Crosslinking effect |
| Example 1 | The reaction activity is good |
| Example 2 | The reaction activity is good |
| Example 3 | The reaction activity is good |
| Example 4 | The reaction activity is good |
| Example 5 | The reaction activity is good |
| Comparative example 1 | The addition reaction cannot be completed |
| Comparative example 2 | ---- |
As can be seen from Table 2, the crosslinking effect of the products of examples 1-5 is good, but in comparative example 1, because the neutralization process is complex, the solid-liquid phase separation needs to be carried out by adopting a settling or filtering mode after the reaction is finished, because the filtration is difficult, the yield is low, the reaction byproducts are more, and the crosslinking effect is poor; in comparative example 2, acidic resin beads were used as the catalyst, but the reaction apparatus was a fixed bed, and the flow rate of the material was very slow due to the high viscosity during the reaction, so that no reaction product could be obtained.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the scope of the present invention, which is defined by the appended claims.
Claims (8)
1. A method for preparing a polysiloxane crosslinking agent; the method is characterized by comprising the following steps:
(1) Feeding: the composition comprises the following raw materials in parts by weight: 1-2 parts of hexamethyldisiloxane and 2-30 parts of high hydrogen-containing silicone oil; 20-120 parts of siloxane mixed ring body;
(2) Telomerization: the raw materials are put into a reaction kettle for equilibrium reaction, acidic resin ball catalyst is filled in the reaction kettle, the reaction temperature in the reaction kettle is 80-90 ℃, and the reaction time is 4-8 hours;
(3) Removing low molecules: after the reaction in the reaction kettle is finished, conveying the materials in the reaction kettle to a low-molecular removal device for removing low molecules;
(4) Cooling and packaging: cooling the polysiloxane cross-linking agent product with the low molecular weight removed, and packaging the obtained product;
and (3) arranging an outer jacket on the outer wall of the reaction kettle in the step (2), arranging a fine-meshed inner jacket on the inner wall of the reaction kettle, arranging a fine-meshed cavity baffle plate on the circumference of the inner jacket, and filling acid resin balls in the inner jacket and the cavity baffle plate.
2. The method for preparing a polysiloxane crosslinking agent according to claim 1, wherein the capping agent in step (1) is hexamethyldisiloxane.
3. The method of claim 1, wherein the silicone mixed ring of step (1) is subjected to moisture removal prior to being added to the reaction vessel.
4. The method for preparing a polysiloxane crosslinking agent according to claim 1, wherein the acidic resin beads in step (2) are cationic acidic resin catalysts, the particle size of the acidic resin beads is 500-1000 μm, and the pore diameter of the pores is 300 μm.
5. The method for preparing a polysiloxane crosslinking agent according to claim 4, wherein the filling volume of the acidic resin beads in step (2) is 5-15% of the total volume of the reaction vessel.
6. The method for preparing a polysiloxane crosslinking agent according to claim 1, wherein the low molecular weight removal equipment in step (3) is a thin film evaporator or a distillation column.
7. The method for preparing a polysiloxane crosslinking agent according to claim 6, wherein the vacuum degree of the low molecular weight removal device in the step (3) is-0.099 MPa to-0.09 MPa, and the temperature of the low molecular weight removal device is 140-150 ℃.
8. The method for preparing a polysiloxane crosslinking agent according to claim 1, wherein the cooling in step (4) is to cool the product of the polysiloxane crosslinking agent with low molecular weight removed to room temperature.
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| CN202111064856.1A CN114133567B (en) | 2021-09-11 | 2021-09-11 | Preparation method of polysiloxane cross-linking agent |
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| CN110577646A (en) * | 2018-06-11 | 2019-12-17 | 苏州汉圭化工科技有限公司 | Production equipment of low-hydrogen-content silicone oil and synthetic method of low-hydrogen-content silicone oil |
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