CN114456384A - Preparation method of ultra-high molecular weight polydimethylsiloxane - Google Patents
Preparation method of ultra-high molecular weight polydimethylsiloxane Download PDFInfo
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- CN114456384A CN114456384A CN202210195427.6A CN202210195427A CN114456384A CN 114456384 A CN114456384 A CN 114456384A CN 202210195427 A CN202210195427 A CN 202210195427A CN 114456384 A CN114456384 A CN 114456384A
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- 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
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- C08G77/08—Preparatory processes characterised by the catalysts used
Abstract
The invention relates to a preparation method of ultra-high molecular weight polydimethylsiloxane, belonging to the technical field of organic silicon, and comprising the following steps of firstly, treating silicon rubber waste to obtain a base material; adding a base material, benzenesulfonic acid and a solvent into a cracking reaction kettle to obtain DMC crude oil; second step, rearrangement: adding DMC crude oil into a rearrangement kettle for rearrangement; step three, polymerization: carrying out nitrogen bubbling cooling on the rearranged DMC, decoloring, deodorizing, filtering, dehydrating, adding alkali gel, and heating for polymerization; step four, neutralization: and after the polymerization reaction is finished, adding a neutralizing agent, and introducing nitrogen to react. The invention can make the product produced by the cracking material reach the quality of the DMC raw material production in the monomer plant by controlling the raw material selection and optimizing the production process, thereby not only reducing the production cost of the product, but also recycling the leftover materials of the non-degradable silica gel products, improving the added value of the product and being beneficial to environmental protection.
Description
Technical Field
The invention belongs to the technical field of organic silicon, and particularly relates to a preparation method of ultra-high molecular weight polydimethylsiloxane.
Background
The polydimethylsiloxane with the ultrahigh molecular weight is the polydimethylsiloxane terminated by a small amount of hydroxyl groups and is used as the main component of the textile auxiliary smoothing agent, and compared with the traditional smoothing agent, the polydimethylsiloxane has the advantages of good continuous film forming property, very obvious smoothness, large film thickness, high refractive index, remarkable brightness of fabrics, fine and smooth hand feeling and no hand adhesion, and is widely used for the after-finishing of fabrics such as cotton, wool, blended fabrics and the like.
The existing polydimethylsiloxane with ultrahigh molecular weight in the market is produced by dimethyl siloxane mixed ring body (DMC) obtained by hydrolyzing and cracking organosilicon monomer dimethyl dichlorosilane, and the cost is relatively high; the method for producing the organic silicon by cracking the waste silicon rubber and recycling the leftover materials of the silicon rubber products is a common method in the prior art, but the method has the conditions of low product purity, unstable product quality and the like. For example, the following problems are involved in the disposal of the reclaimed materials: silicone rubber can be broken in high pressure water vapor to depolymerize siloxane bonds to siloxane oligomers, with low yields of dimethyl siloxane mixed rings (DMC).
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a preparation method of ultra-high molecular weight polydimethylsiloxane.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of ultra-high molecular weight polydimethylsiloxane comprises the following steps:
the first step, pretreatment: treating the silicon rubber waste: cleaning, cutting into pieces, drying and crushing to obtain a base material; cracking the obtained base material: adding a base material, benzenesulfonic acid and a solvent into a cracking reaction kettle, reducing the decomposition and carrying-out of a cross-linking agent in a product, and reducing the carrying-out of trifunctional group substances, namely methyl trimethoxy, methyl triethoxy and products with amino groups as much as possible; heating to 150 ℃ and 160 ℃, keeping the vacuum degree at-0.098 kPa, keeping the reaction time at 3-5h, reducing the cracking temperature as much as possible, reducing impurities carried out by high-temperature cracking as much as possible, further improving the product purity, and obtaining DMC (dimethyl siloxane mixed ring body) crude oil after water and acid separation;
second step, rearrangement: adding DMC crude oil into a rearrangement kettle, then adding a filler and an alkaline catalyst, heating to 145-155 ℃ for reaction, setting reflux, and facilitating collection of D4 (octamethylcyclotetrasiloxane); until the content of D3 (hexamethylcyclotrisiloxane) is below 1%, the content of D4 (octamethylcyclotetrasiloxane) is above 80%, the content of D5 (decamethylcyclopentasiloxane) is below 15%, and the content of D6 (decadimethylcyclohexasiloxane) is below 4%, filtering to obtain rearranged DMC;
step three, polymerization: reducing the temperature of rearranged DMC by nitrogen bubbling for 4-6h, decoloring by active carbon, deodorizing, filtering, heating to 90-100 ℃, dehydrating for 2h, adding alkali gel, wherein the self-made alkali gel can improve the dispersibility in the system, ensuring that the polymerization process can be completed uniformly, heating to 140-160 ℃ for polymerization reaction for 2h, heating to 150-160 ℃ for continuous polymerization reaction for 2h, and increasing the polymerization time to make the molecular weight distribution narrower as much as possible, thereby improving the product quality; and introducing water vapor to depolymerize to make the viscosity of the polymer reach 500 million CP and the molecular weight of the polymer about 40 million, so that the use requirement of the smoothing agent can be met.
Step four, neutralization: after the polymerization reaction is finished, adding a neutralizer, introducing nitrogen, carrying out neutralization reaction for 2h at the temperature of 150-.
Further, the filler is prepared by the following steps:
step S11, mixing dopamine hydrochloride with water, adding a citric acid/sodium citrate buffer solution, maintaining the pH value of the reaction to be 5.0-6.0, adding activated carbon powder under the condition of keeping out of the sun, stirring and reacting for 24 hours at 25 ℃, and filtering and drying after the reaction is finished to obtain dopamine modified activated carbon; under an acidic condition, dopamine can form a single dopamine layer on the surface of the activated carbon, and the single dopamine layer has amino groups to provide reaction sites for subsequent reactions;
and step S12, adding terephthalaldehyde and dopamine modified activated carbon into a toluene solution, heating and refluxing for 2 hours under the protection of nitrogen, and filtering and drying after refluxing to obtain the filler. And performing nucleophilic addition reaction on aldehyde group on the terephthalaldehyde and amino group on the dopamine modified activated carbon to form a Schiff base structure, thereby obtaining the filler. And a certain amount of filler prepared by taking the activated carbon as a raw material is added, so that oxidation of silicon-oxygen bonds caused by high temperature is avoided, the quality of products in a rearrangement process is improved, and the yield of the products is further improved.
Further, in the step S11, the mass ratio of the dopamine hydrochloride to the activated carbon powder is 0.8: 2; in the step S12, the dosage mass ratio of the terephthalaldehyde to the dopamine modified activated carbon is 0.2: 4.
further, the alkaline catalyst is potassium hydroxide, and the addition amount of the alkaline catalyst is 0.8-1.5% of the mass of the DMC crude oil. The potassium hydroxide belongs to alkali metal hydroxide, and is compounded with the filler, so that the stability of a reaction system can be improved, and the temperature required by the reaction can be reduced.
Further, the alkali glue is prepared by the following steps:
under the protection condition of nitrogen, the mass ratio of 100: 1, mixing DMC and potassium hydroxide, heating up to maintain the temperature of 100-120 ℃, stirring for 2-3h, and cooling to obtain the alkali glue.
Further, the neutralizing agent is prepared by the following steps:
under the protection condition of nitrogen, the mass ratio of 100: 1, mixing DMC and phosphoric acid, heating up to maintain 70-75 ℃, stirring for 2-3h, and cooling to obtain a neutralizer.
Further, the silicon rubber waste is one of dimethyl silicon rubber, vinyl silicon rubber, phenyl silicon rubber and ethyl silicon rubber.
Furthermore, the addition amount of the benzenesulfonic acid is 2-8% of the mass of the base material.
Further, the solvent is one of phenyl ether and tetraethylene glycol dimethyl ether.
Furthermore, the addition amount of the alkali gum is 0.3-0.5% of the mass of the rearranged DMC; the addition amount of the neutralizer is 1.1-1.3 times of the mass of the alkali glue.
The invention has the beneficial effects that:
the invention can make the product produced by cracking material reach the quality of DMC material production in monomer factory by controlling the raw material selection and optimizing the production process, which can reduce the production cost and recycle the leftover material of non-degradable silica gel product, improve the added value and is beneficial to environmental protection.
The dopamine forms a monolayer dopamine layer under an acidic condition, the monolayer dopamine has amino groups, the melting point temperature range of the dopamine is 219-221 ℃, the dopamine reaches the boiling point temperature at 336-338 ℃, the dopamine is easily soluble in water, and the aldehyde group on the terephthalaldehyde and the amino group on the dopamine modified activated carbon undergo nucleophilic addition reaction to obtain the filler. And a certain amount of filler prepared by taking the activated carbon as a raw material is added, so that oxidation of silicon-oxygen bonds caused by high temperature is avoided, the quality of products in a rearrangement process is improved, and the yield of the products is further improved. The N atom on the hybrid orbit in the Schiff base structure has lone pair electrons, and the stability of the whole solution can be improved after the N atom is compounded with the alkali metal hydroxide, so that the required temperature is reduced, the dosage of the alkali metal hydroxide is greatly reduced, the reaction efficiency is improved, and the energy consumption is effectively reduced.
The molecular weight distribution is narrower as much as possible by prolonging the polymerization time in the polymerization reaction process, and the product quality is improved. And introducing water vapor to depolymerize to make the viscosity of the polymer reach 500 million CP and the molecular weight of the polymer about 40 million, so that the use requirement of the smoothing agent can be met.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a filler:
step S11, mixing dopamine hydrochloride with water, then adding citric acid/sodium citrate buffer solution, maintaining the pH value of the reaction to be 5.0-6.0, adding activated carbon powder under the condition of keeping out of the sun, stirring and reacting for 24 hours at 25 ℃, and after the reaction is finished, filtering and drying to obtain dopamine modified activated carbon; the dosage mass ratio of the dopamine hydrochloride to the activated carbon powder is 0.8: 2;
and step S12, adding terephthalaldehyde and dopamine modified activated carbon into a toluene solution, heating and refluxing for 2 hours under the condition of nitrogen protection, and filtering and drying after refluxing to obtain the filler. The dosage mass ratio of the terephthalaldehyde to the dopamine modified activated carbon is 0.2: 4.
example 2
Preparing alkali glue:
under the protection of nitrogen, according to the mass ratio of 100: 1, mixing DMC and potassium hydroxide, heating up and maintaining the temperature at 100 ℃, stirring for 3 hours, and cooling to obtain the alkali glue.
Preparing a neutralizing agent:
under the protection condition of nitrogen, the mass ratio of 100: 1, mixing DMC and phosphoric acid, heating up and maintaining the temperature at 70 ℃, stirring for 3 hours, and cooling to obtain a neutralizer.
Example 3
Preparing alkali glue:
under the protection condition of nitrogen, the mass ratio of 100: 1, mixing DMC and potassium hydroxide, heating up and maintaining 120 ℃, stirring for 2 hours, and cooling to obtain the alkali glue.
Preparation of a neutralizing agent:
under the protection of nitrogen, according to the mass ratio of 100: 1, mixing DMC and phosphoric acid, heating up and maintaining the temperature at 75 ℃, stirring for 2 hours, and cooling to obtain a neutralizer.
Example 4
A preparation method of ultra-high molecular weight polydimethylsiloxane comprises the following steps:
the first step, pretreatment: treating the dimethyl silicone rubber waste: cleaning, cutting into pieces, drying and crushing to obtain a base material; cracking the obtained base material: adding a base material, benzenesulfonic acid and phenyl ether into a cracking reaction kettle, heating to 150 ℃, keeping the vacuum degree at-0.098 kPa, reacting for 5h, and separating water and acid to obtain DMC (dimethyl siloxane mixed ring body) crude oil;
second step, rearrangement: adding DMC crude oil into a rearrangement kettle, then adding the filler prepared in the example 1 and potassium hydroxide, heating to 145 ℃ for reflux reaction, and conveniently collecting D4 (octamethylcyclotetrasiloxane); until the content of D3 (hexamethylcyclotrisiloxane) is below 1%, the content of D4 (octamethylcyclotetrasiloxane) is above 80%, the content of D5 (decamethylcyclopentasiloxane) is below 15%, and the content of D6 (decadimethylcyclohexasiloxane) is below 4%, filtering to obtain rearranged DMC;
step three, polymerization: and (3) carrying out nitrogen bubbling on the rearranged DMC, cooling for 4h, decoloring by using activated carbon, deodorizing, filtering, heating to 100 ℃, carrying out dehydration treatment for 2h, adding the alkali glue prepared in the embodiment 2, heating to 140 ℃, carrying out polymerization reaction for 2h, and heating to 150 ℃, and continuing the polymerization reaction for 2 h.
Step four, neutralization: after the polymerization reaction is finished, adding the neutralizing agent prepared in the example 2, introducing nitrogen, carrying out neutralization reaction for 2 hours at the temperature of 150 ℃, after the neutralization is finished, pressing the material into a low molecular weight remover by using the nitrogen for removing the low molecular weight, wherein the low molecular weight remover adopts a pattern plate form, and drawing the material into filaments to obtain the ultra-high molecular weight polydimethylsiloxane.
Wherein the addition amount of the potassium hydroxide is 0.8 percent of the mass of the DMC crude oil; the addition amount of the benzenesulfonic acid is 2% of the mass of the base material. The addition amount of the alkali gum is 0.3 percent of the mass of the rearranged DMC; the addition amount of the neutralizing agent is 1.1 times of the mass of the alkali glue.
Example 5
A preparation method of ultra-high molecular weight polydimethylsiloxane comprises the following steps:
the first step, pretreatment: treating the dimethyl silicone rubber waste: cleaning, cutting into pieces, drying and crushing to obtain a base material; cracking the obtained base material: adding a base material, benzenesulfonic acid and phenylate into a cracking reaction kettle, heating to 155 ℃, controlling the vacuum degree to be-0.098 kPa, controlling the reaction time to be 4h, and obtaining DMC (dimethyl siloxane mixed ring body) crude oil after water and acid are separated;
second step, rearrangement: adding DMC crude oil into a rearrangement kettle, then adding the filler prepared in the example 1 and potassium hydroxide, heating to 150 ℃, and carrying out reflux reaction, so as to facilitate the collection of D4 (octamethylcyclotetrasiloxane); until the content of D3 (hexamethylcyclotrisiloxane) is below 1%, the content of D4 (octamethylcyclotetrasiloxane) is above 80%, the content of D5 (decamethylcyclopentasiloxane) is below 15%, and the content of D6 (decadimethylcyclohexasiloxane) is below 4%, filtering to obtain rearranged DMC;
step three, polymerization: and (3) carrying out nitrogen bubbling on the rearranged DMC, cooling for 5h, decoloring by using activated carbon, deodorizing, filtering, heating to 95 ℃, carrying out dehydration treatment for 2h, adding the alkali glue prepared in the embodiment 2, heating to 145 ℃, carrying out polymerization reaction for 2h, and heating to 155 ℃ for continuing the polymerization reaction for 2 h.
Step four, neutralization: after the polymerization reaction, the neutralizer prepared in the example 2 is added, nitrogen is introduced, the neutralization reaction is carried out for 2 hours at the temperature of 155 ℃, after the neutralization is finished, the material is pressed into a low molecular weight remover by the nitrogen for removing the low molecular weight, the low molecular weight remover adopts a pattern plate form, and the material is drawn into filaments, so that the ultra-high molecular weight polydimethylsiloxane is obtained.
Wherein the addition amount of the potassium hydroxide is 1 percent of the mass of the DMC crude oil; the addition amount of the benzenesulfonic acid is 5 percent of the mass of the base material; the addition amount of the alkali gum is 0.4 percent of the mass of the rearranged DMC; the addition amount of the neutralizing agent is 1.2 times of the mass of the alkali glue.
Example 6
A preparation method of ultra-high molecular weight polydimethylsiloxane comprises the following steps:
the first step, pretreatment: treating the dimethyl silicone rubber waste: cleaning, cutting into pieces, drying and crushing to obtain a base material; cracking the obtained base material: adding a base material, benzenesulfonic acid and tetraethylene glycol dimethyl ether into a cracking reaction kettle, heating to 160 ℃, keeping the vacuum degree at-0.098 kPa, reacting for 5h, and separating water and acid to obtain DMC (dimethyl siloxane mixed ring body) crude oil;
second step, rearrangement: adding DMC crude oil into a rearrangement kettle, then adding the filler prepared in the example 1 and potassium hydroxide, heating to 155 ℃, and carrying out reflux reaction, so that D4 (octamethylcyclotetrasiloxane) can be conveniently collected; until the content of D3 (hexamethylcyclotrisiloxane) is below 1%, the content of D4 (octamethylcyclotetrasiloxane) is above 80%, the content of D5 (decamethylcyclopentasiloxane) is below 15%, and the content of D6 (decadimethylcyclohexasiloxane) is below 4%, filtering to obtain rearranged DMC;
step three, polymerization: and (3) carrying out nitrogen bubbling cooling on the rearranged DMC for 6h, decoloring by using activated carbon, deodorizing, filtering, heating to 90 ℃, carrying out dehydration treatment for 2h, adding the alkali glue prepared in the embodiment 3, heating to 150 ℃, carrying out polymerization reaction for 2h, and heating to 160 ℃, and continuing the polymerization reaction for 2 h.
Step four, neutralization: after the polymerization reaction, the neutralizer prepared in the example 3 is added, nitrogen is introduced, the neutralization reaction is carried out for 2 hours at the temperature of 160 ℃, after the neutralization is finished, the material is pressed into a low molecular weight remover by the nitrogen for removing the low molecular weight, the low molecular weight remover adopts a pattern plate form, and the material is drawn into filaments, so that the ultra-high molecular weight polydimethylsiloxane is obtained.
Wherein the addition amount of the potassium hydroxide is 1.5 percent of the mass of the DMC crude oil; the addition amount of the benzenesulfonic acid is 8 percent of the mass of the base material; the addition amount of the alkali gum is 0.5 percent of the mass of the rearranged DMC; the addition amount of the neutralizer is 1.3 times of the mass of the alkali glue.
Comparative example 1
The filler in example 5 was replaced by activated carbon, and the remaining raw materials and preparation process were kept unchanged. The content of D4 (octamethylcyclotetrasiloxane) is less than 80%; the rearrangement temperature was raised to 170 ℃ and the D4 (octamethylcyclotetrasiloxane) content reached 80%, but the yield was significantly reduced.
Comparative example 2
Compared with example 5, no filler is added, and the rest of raw materials and the preparation process are unchanged. The content of D4 (octamethylcyclotetrasiloxane) is less than 80%, the rearrangement temperature is increased to 170 ℃, and the content cannot reach 80%.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (10)
1. A preparation method of ultra-high molecular weight polydimethylsiloxane is characterized by comprising the following steps:
firstly, treating silicon rubber waste to obtain a base material; adding the base material, benzenesulfonic acid and solvent into a cracking reaction kettle, heating to 150-160 ℃, controlling the vacuum degree to be-0.098 kPa, and controlling the reaction time to be 3-5h to obtain DMC crude oil;
second step, rearrangement: adding DMC crude oil into a rearrangement kettle, then adding a filler and an alkaline catalyst, and heating to 145-155 ℃ for reflux reaction; filtering to obtain rearranged DMC;
step three, polymerization: cooling rearranged DMC by nitrogen bubbling for 4-6h, decoloring by active carbon, deodorizing, filtering, heating to 90-100 ℃, dehydrating for 2h, adding alkali glue, heating to 140-160 ℃ for polymerization reaction for 2h, and heating to 150-160 ℃ for polymerization reaction for 2 h;
step four, neutralization: after the polymerization reaction is finished, adding a neutralizer, introducing nitrogen, and carrying out neutralization reaction for 2h at the temperature of 150-.
2. The method of claim 1, wherein the reaction is performed under reflux until the content of D3 is less than 1%, the content of D4 is more than 80%, the content of D5 is less than 15%, and the content of D6 is less than 4%, and the reaction is completed.
3. The method of claim 1, wherein after the neutralization in the fourth step, the material is pressed into a low molecular weight remover with nitrogen gas to remove the low molecular weight, and the material is drawn into a filament to obtain the product.
4. The method of claim 1, wherein the filler is prepared by the steps of:
step S11, mixing dopamine hydrochloride with water, adding a citric acid/sodium citrate buffer solution, maintaining the pH value of the reaction to be 5.0-6.0, adding activated carbon powder under the condition of keeping out of the sun, and stirring and reacting for 24 hours at 25 ℃ to obtain dopamine modified activated carbon;
step S12, adding terephthalaldehyde and dopamine modified activated carbon into a toluene solution, and heating and refluxing for 2 hours under the protection of nitrogen to obtain a filler; the addition amount of the filler is 5 percent of the mass of the DMC crude oil.
5. The method for preparing ultra-high molecular weight polydimethylsiloxane as claimed in claim 1, wherein the basic catalyst is potassium hydroxide, and the addition amount of the basic catalyst is 0.8-1.5% of the mass of the DMC raw oil.
6. The method of claim 1, wherein the alkali gel is prepared by the steps of:
under the protection condition of nitrogen, the mass ratio of 100: 1, mixing DMC and potassium hydroxide, heating up to maintain the temperature of 100-120 ℃, stirring for 2-3h, and cooling to obtain the alkali glue.
7. The method of claim 1, wherein the neutralizing agent is prepared by the steps of:
under the protection condition of nitrogen, the mass ratio of 100: 1, mixing DMC and phosphoric acid, heating up to maintain 70-75 ℃, stirring for 2-3h, and cooling to obtain a neutralizer.
8. The method of claim 1, wherein the benzene sulfonic acid is added in an amount of 2-8% by mass based on the mass of the base material.
9. The method of claim 1, wherein the solvent is one of phenyl ether and tetraglyme.
10. The method of claim 1, wherein the amount of the alkali gum added is 0.3-0.5% of the mass of the rearranged DMC; the addition amount of the neutralizer is 1.1-1.3 times of the mass of the alkali glue.
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| JP2009144132A (en) * | 2007-07-09 | 2009-07-02 | Toray Ind Inc | Method for producing polylactic acid-based resin |
| CN101649047A (en) * | 2008-08-14 | 2010-02-17 | 扬州宏远化工新材料有限公司 | Simethicone |
| CN102140170A (en) * | 2010-12-28 | 2011-08-03 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of high-molecular-weight permethyl silicone oil |
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- 2022-03-01 CN CN202210195427.6A patent/CN114456384A/en active Pending
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| JP2009144132A (en) * | 2007-07-09 | 2009-07-02 | Toray Ind Inc | Method for producing polylactic acid-based resin |
| CN101338034A (en) * | 2008-06-06 | 2009-01-07 | 浙江新安化工集团股份有限公司 | Novel process for synthesizing 107 silicon rubber |
| CN101649047A (en) * | 2008-08-14 | 2010-02-17 | 扬州宏远化工新材料有限公司 | Simethicone |
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Application publication date: 20220510 |