CN110938207B - Preparation method of hydrogen-containing silicone oil - Google Patents
Preparation method of hydrogen-containing silicone oil Download PDFInfo
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- CN110938207B CN110938207B CN201911253965.0A CN201911253965A CN110938207B CN 110938207 B CN110938207 B CN 110938207B CN 201911253965 A CN201911253965 A CN 201911253965A CN 110938207 B CN110938207 B CN 110938207B
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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
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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
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
Abstract
The invention discloses a preparation method of hydrogen-containing silicone oil, relating to the technical field of silicone oil preparation, and the key point of the technical scheme is the preparation method of the hydrogen-containing silicone oil, which comprises the following steps: and (2) taking cyclosiloxane as a reaction monomer, adding a hydrogen end-capping agent, carrying out polymerization reaction under the action of a modified activated clay catalyst, filtering the modified activated clay catalyst after the polymerization reaction is finished, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil. The activated clay is used as the catalyst in the catalytic equilibrium method, so that the use amount of the catalyst is reduced, the production cost is reduced, the post-treatment is mild, the operation is easy, and the production process is simplified.
Description
Technical Field
The invention relates to the technical field of preparation of silicone oil, in particular to a preparation method of hydrogen-containing silicone oil.
Background
Silicone oils generally refer to linear silicone products which remain liquid at room temperature, hydrogen-containing silicone oils being an important class of silicone oil products, the molecular formula of which is Me3SiO(MeHSiO)m(Me2SiO)nSiMe3The siloxane main chain of the modified block silicone oil has active group hydrogen, has higher activity, can react with various active groups, and is often used as a raw material for synthesizing the block modified silicone oil and the graft modified silicone oil.
At present, the method for preparing the hydrogen-containing silicone oil mainly comprises three methods, namely an alcoholysis-followed hydrolysis, cohydrolysis condensation method and a catalytic equilibrium method, most of domestic manufacturers adopt the cohydrolysis condensation method to prepare the hydrogen-containing silicone oil at present, but the cohydrolysis condensation method is easy to generate gel during hydrolysis, and has unstable product quality and poor performance; the catalyst balance method adopts end capping agent, so that the product performance is more stable, and the method adopts D4 (octamethylcyclotetrasiloxane) and hydrogen-containing double-end-cap (tetramethyldihydro-disiloxane) as raw materials to perform polymerization reaction under the action of catalyst. In the prior art, patent application publication No. CN106432731A discloses a hydrogen-containing silicone oil with double ends and a preparation method thereof, wherein the preparation method comprises the following steps: 450kg of octamethylcyclotetrasiloxane 350-plus and 4-9kg of hydrogen-containing double-end enclosure are sequentially added into an enamel reaction kettle, 8-15kg of concentrated sulfuric acid is added after stirring, the temperature is kept at 20-50 ℃ for reaction for 4-8h, 12-18kg of soda is slowly added in batches for system pH adjustment, the stirring is continued for 2-5h, and then discharging and standing sedimentation are carried out, so that the hydrogen-containing silicone oil at the two ends is obtained.
Concentrated sulfuric acid as a catalyst in the preparation of hydrogen-containing silicone oil can improve the reaction rate, but the concentrated sulfuric acid is a strong corrosive mineral acid, so the operation risk is high, the purchase is difficult, the post-treatment irritation is strong, a large amount of solid residues are caused, and the process difficulty is increased.
Disclosure of Invention
The invention aims to provide a preparation method of hydrogen-containing silicone oil, which uses activated clay as a catalyst, greatly reduces the using amount of the catalyst, reduces the production cost, has mild post-treatment and easy operation, and simplifies the production process.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of hydrogen-containing silicone oil comprises the following steps: and (2) taking cyclosiloxane as a reaction monomer, adding a hydrogen end-capping agent, carrying out polymerization reaction under the action of a modified activated clay catalyst, filtering the modified activated clay catalyst after the polymerization reaction is finished, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil.
By adopting the technical scheme, the activated clay is used as the catalyst in the catalytic equilibrium method, so that the use amount of the catalyst is reduced, the production cost is reduced, the post-treatment is mild, the operation is easy, and the production process is simplified.
Further, the hydrogen-terminated end-capping agent is 1,1,3, 3-tetramethyl dihydro disiloxane; the cyclosiloxane is octamethylcyclotetrasiloxane.
Further, the method specifically comprises the following steps:
s1, taking 29-75 parts by weight of hydrogen-terminated end-capping agent and 1900 parts by weight of cyclosiloxane, adding modified activated clay catalyst while stirring, heating to 80 ℃, and preserving heat for 8-12 hours to perform polymerization reaction;
and S2, after the polymerization reaction is finished, filtering the modified activated clay catalyst, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil.
By adopting the technical scheme, the polymerization degree of the hydrogen-containing silicone oil can be controlled by controlling the dosage of the hydrogen-terminated end-capping reagent, and the operation is convenient.
Further, the activated clay catalyst is prepared by the following method: taking 100 parts of water, adding 10-15 parts of phosphotungstic acid, and uniformly stirring to obtain a phosphotungstic acid solution; adding 30-40 parts of activated clay into the phosphotungstic acid solution, and stirring for 1-3 hours at the temperature of 80-90 ℃ to obtain activated clay suspension; thirdly, decompressing the activated clay suspension to-0.09 MPa, maintaining for 30-40min to obtain the prefabricated activated clay, washing the prefabricated activated clay by water, and roasting at the temperature of 160-170 ℃ for 4-6h to obtain the modified activated clay catalyst.
Through adopting above-mentioned technical scheme, traditional activated clay has fine catalytic action to the polymerization of hydrogen-containing silicone oil, but compares in concentrated sulfuric acid catalyst, and its yield of reaction is slightly low, through carrying out modification treatment to activated clay, can increase activated clay's interlamellar spacing and lipophilicity, improves its catalytic efficiency, reduces its quantity.
Further, the stirring speed in the step two is 100-200 r/min.
By adopting the technical scheme, the phosphotungstic acid solution and the activated clay suspension can be uniformly mixed at the speed of 100-200r/min, so that the catalytic efficiency of the modified activated clay catalyst is improved.
Further, after the polymerization reaction in S2 is finished, 10-15 parts of modified diatomite filter aid is added for circular filtration until the filtrate is clear and transparent.
By adopting the technical scheme, the activated clay catalyst has excellent catalytic efficiency, but has smaller particles due to the solid powder, is difficult to separate after being mixed with the silicone oil, has stronger adsorption force, and further increases the separation difficulty of the activated clay catalyst and the silicone oil; the modified diatomite filter aid has good adsorption effect on the modified activated clay catalyst, and can quickly filter the modified activated clay catalyst, so that the technological process is easier to operate.
Further, the modified diatomite filter aid is prepared by adopting the following method: (1) taking 100 parts of water, adding 10-15 parts of ferric chloride, and uniformly stirring to obtain a ferric chloride solution; (2) adding 50-60 parts of diatomite into the ferric chloride solution, and stirring for 1-2 hours at the temperature of 60-80 ℃ to obtain a diatomite suspension; (3) and settling and filtering the diatomite suspension to obtain diatomite precipitate, washing the diatomite precipitate with water, roasting at the temperature of 130-140 ℃ for 3-5h to obtain modified diatomite, and granulating the modified diatomite to obtain the modified diatomite filter aid.
By adopting the technical scheme, the modified diatomite filter aid prepared by modifying diatomite by introducing iron ions has the advantages of large specific surface area and strong adsorption force, has good adsorption effect on the modified activated clay catalyst, can quickly adsorb and filter the modified activated clay catalyst, and greatly simplifies the operation process.
Further, the granulation in step (3) is specifically performed as follows: adding sodium carbonate, kaolin, sodium bicarbonate, zeolite powder and sodium ethylene diamine tetra methylene phosphonate into the modified diatomite, adding an aqueous solution of polyvinyl alcohol while stirring, carrying out rolling granulation to obtain granules, and drying and roasting the granules to obtain the modified diatomite.
By adopting the technical scheme, the modified diatomite filter aid prepared from the modified diatomite, sodium carbonate, kaolin, sodium bicarbonate, zeolite powder, ethylene diamine tetra (methylene phosphonic acid) sodium and polyvinyl alcohol has good adsorption effect on the modified activated clay catalyst, is easy to separate from silicone oil, is simple to operate, and reduces the production cost.
In summary, compared with the prior art, the invention has the following beneficial effects:
1. the activated clay is used as the catalyst in the catalytic equilibrium method, so that the use amount of the catalyst is reduced, the production cost is reduced, the post-treatment is mild and easy to operate, and the production process is simplified;
2. although the traditional activated clay has a good catalytic effect on the polymerization reaction of hydrogen-containing silicone oil, compared with a concentrated sulfuric acid catalyst, the yield of the reaction is slightly low, and the interlayer spacing and lipophilicity of the activated clay can be increased by modifying the activated clay, so that the catalytic efficiency is improved, and the dosage is reduced;
3. the modified diatomite filter aid prepared by modifying diatomite by introducing iron ions has the advantages of large specific surface area and strong adsorption force, has good adsorption effect on the modified activated clay catalyst, can quickly adsorb and filter the modified activated clay catalyst, and greatly simplifies the operation process.
Detailed Description
The present invention will be described in further detail below.
Preparation example of modified activated Clay catalyst
Preparation example 1 of modified activated clay catalyst: firstly, taking 100kg of water, adding 12.5kg of phosphotungstic acid, and uniformly stirring to obtain a phosphotungstic acid solution; adding 35kg of activated clay into the phosphotungstic acid solution, and stirring for 2 hours at the temperature of 85 ℃ at the speed of 150r/min to obtain activated clay suspension; thirdly, decompressing the activated clay suspension to-0.09 MPa, maintaining for 35min to obtain the prefabricated activated clay, washing the prefabricated activated clay with water, and roasting at 165 ℃ for 5h to obtain the modified activated clay catalyst.
Preparation example 2 of modified activated clay catalyst: taking 100kg of water, adding 10kg of phosphotungstic acid, and uniformly stirring to obtain a phosphotungstic acid solution; adding 30kg of activated clay into the phosphotungstic acid solution, and stirring for 1h at the temperature of 80-90 ℃ and the speed of 100r/min to obtain activated clay suspension; thirdly, decompressing the activated clay suspension to-0.09 MPa, maintaining for 30min to obtain the prefabricated activated clay, washing the prefabricated activated clay with water, and roasting for 4h at the temperature of 160 ℃ to obtain the modified activated clay catalyst.
Preparation example 3 of modified activated clay catalyst: taking 100kg of water, adding 15kg of phosphotungstic acid, and uniformly stirring to obtain a phosphotungstic acid solution; adding 40kg of activated clay into the phosphotungstic acid solution, and stirring for 3 hours at the temperature of 90 ℃ at the speed of 200r/min to obtain activated clay suspension; and thirdly, decompressing the activated clay suspension to-0.09 MPa, maintaining for 40min to obtain the prefabricated activated clay, washing the prefabricated activated clay by using water, and roasting at the temperature of 170 ℃ for 6h to obtain the modified activated clay catalyst.
Preparation example 4 of modified activated clay catalyst: the phosphotungstic acid was replaced with an equal amount of aluminum trichloride.
Preparation example of modified diatomaceous earth Filter aid diatomaceous earth in the following preparation examples was selected from 110 model diatomaceous earth raw ore provided by Guishou county Xin mineral processing plant; the polyvinyl alcohol is selected from the group consisting of 2488 model number polyvinyl alcohol available from July chemical Co., Ltd.
Preparation example 1 of modified diatomaceous earth Filter aid: (1) taking 100kg of water, adding 12.5kg of ferric chloride, and uniformly stirring to obtain a ferric chloride solution; (2) adding 55kg of diatomite into the ferric chloride solution, and stirring for 1.5h at the temperature of 70 ℃ to obtain a diatomite suspension; (3) settling and filtering the diatomite suspension to obtain diatomite precipitate, washing the diatomite precipitate with water, and roasting at the temperature of 135 ℃ for 4 hours to obtain modified diatomite; (4) adding 2kg of ethylene diamine tetra methylene phosphonic acid sodium into modified diatomite in a spray mode, then adding 6kg of sodium carbonate, 6kg of kaolin, 5kg of sodium bicarbonate and 3kg of zeolite powder, adding 10 wt% of polyvinyl alcohol aqueous solution while stirring, wherein the addition amount of the polyvinyl alcohol aqueous solution is 30kg, carrying out rolling granulation to obtain granules with the particle size of 3-5mm, placing the granules at the temperature of 100 ℃, drying for 2h, placing the granules at the temperature of 700 ℃, and roasting for 5h to obtain the modified diatomite filter aid.
Preparation example 2 of modified diatomaceous earth Filter aid: (1) taking 100kg of water, adding 10kg of ferric chloride, and uniformly stirring to obtain a ferric chloride solution; (2) adding 50kg of diatomite into the ferric chloride solution, and stirring for 1h at the temperature of 60 ℃ to obtain a diatomite suspension; (3) settling and filtering the diatomite suspension to obtain diatomite precipitate, washing the diatomite precipitate with water, and roasting at the temperature of 130 ℃ for 3 hours to obtain modified diatomite; (4) adding 2kg of ethylene diamine tetra methylene phosphonic acid sodium into modified diatomite in a spray mode, then adding 6kg of sodium carbonate, 6kg of kaolin, 5kg of sodium bicarbonate and 3kg of zeolite powder, adding 10 wt% of polyvinyl alcohol aqueous solution while stirring, wherein the addition amount of the polyvinyl alcohol aqueous solution is 30kg, carrying out rolling granulation to obtain granules with the particle size of 3-5mm, placing the granules at the temperature of 100 ℃, drying for 2h, placing the granules at the temperature of 700 ℃, and roasting for 5h to obtain the modified diatomite filter aid.
Preparation example 3 of modified diatomaceous earth filter aid: (1) taking 100kg of water, adding 15kg of ferric chloride, and uniformly stirring to obtain a ferric chloride solution; (2) adding 60kg of diatomite into the ferric chloride solution, and stirring for 2 hours at the temperature of 80 ℃ to obtain a diatomite suspension; (3) settling and filtering the diatomite suspension to obtain diatomite precipitate, washing the diatomite precipitate with water, and roasting at 140 ℃ for 5 hours to obtain modified diatomite; (4) adding 2kg of ethylene diamine tetra methylene phosphonic acid sodium into modified diatomite in a spray mode, then adding 6kg of sodium carbonate, 6kg of kaolin, 5kg of sodium bicarbonate and 3kg of zeolite powder, adding 10 wt% of polyvinyl alcohol aqueous solution while stirring, wherein the addition amount of the polyvinyl alcohol aqueous solution is 30kg, carrying out rolling granulation to obtain granules with the particle size of 3-5mm, placing the granules at the temperature of 100 ℃, drying for 2h, placing the granules at the temperature of 700 ℃, and roasting for 5h to obtain the modified diatomite filter aid.
Preparation example 4 of modified diatomaceous earth filter aid: this preparation example differs from preparation example 1 of the modified diatomaceous earth filter aid in that no ferric chloride was added in step (1).
Preparation example 5 of modified diatomaceous earth Filter aid: the difference between this preparation example and preparation example 1 of modified diatomaceous earth filter aid is that zeolite powder and sodium ethylenediamine tetramethylene phosphonate were not added in step (4).
Examples the 1,1,3, 3-tetramethyldihydrodisiloxane in the following examples was selected from 98% 1,1,3, 3-tetramethyldihydrodisiloxane available from Bai Qian chemical Co., Ltd, Shandong; the octamethylcyclotetrasiloxane is octamethylcyclotetrasiloxane provided by Shandong Leong New Material science and technology, Inc.
Example 1: the hydrogen-containing silicone oil is prepared by the following method:
s1, taking 36kg of 1,1,3, 3-tetramethyl dihydro disiloxane and 1900kg of octamethylcyclotetrasiloxane, adding 10kg of modified activated clay catalyst (selected from preparation example 1 of the modified activated clay catalyst) while stirring, heating to 80 ℃, and preserving heat for 8 hours to perform polymerization reaction;
s2, after the polymerization reaction is finished, adding 10kg of modified diatomite filter aid (selected from preparation example 1 of the modified diatomite filter aid), performing circulating filtration until the filtrate is clear and transparent, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil.
Example 2: the hydrogen-containing silicone oil is prepared by the following method:
s1, taking 29kg of 1,1,3, 3-tetramethyl dihydro disiloxane and 1900kg of octamethylcyclotetrasiloxane, adding 10kg of modified activated clay catalyst (selected from preparation example 2 of the modified activated clay catalyst) while stirring, heating to 80 ℃, and preserving heat for 8-12 hours to perform polymerization reaction;
s2, after the polymerization reaction is finished, adding 10kg of modified diatomite filter aid (selected from preparation example 2 of the modified diatomite filter aid), performing circulating filtration until the filtrate is clear and transparent, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil.
Example 3: the hydrogen-containing silicone oil is prepared by the following method:
s1, taking 75kg of 1,1,3, 3-tetramethyl dihydro disiloxane and 1900kg of octamethylcyclotetrasiloxane, adding 10kg of modified activated clay catalyst (selected from preparation example 3 of the modified activated clay catalyst) while stirring, heating to 80 ℃, and preserving heat for 12 hours to perform polymerization reaction;
s2, after the polymerization reaction is finished, adding 10kg of modified diatomite filter aid (selected from preparation example 3 of the modified diatomite filter aid), performing circulating filtration until the filtrate is clear and transparent, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil.
Fourth, comparative example
Comparative example 1: the hydrogen-containing silicone oil is prepared by the following method: taking 36kg of 1,1,3, 3-tetramethyl dihydrodisiloxane and 1900kg of octamethylcyclotetrasiloxane, adding 10kg of 98 mass percent concentrated sulfuric acid while stirring, heating to 30 ℃, preserving heat for 8 hours, and carrying out polymerization reaction; after the polymerization reaction is finished, 15kg of sodium carbonate is added, the mixture is stirred for 2 hours, the temperature is raised to 140 ℃, low-boiling-point substances are pumped out in vacuum until no liquid is pumped out, and clear and transparent liquid is collected to obtain the hydrogen-containing silicone oil.
Comparative example 2: the comparative example is different from example 1 in that the modified activated clay catalyst is a common activated clay provided by Henan Bokelong purification materials Co.
Comparative example 3: this comparative example differs from example 1 in that the modified activated clay catalyst was prepared from modified activated clay catalyst 4.
Comparative example 4: this comparative example differs from example 1 in that the modified diatomaceous earth filter aid was selected from that prepared in preparation example 4.
Comparative example 5: this comparative example differs from example 1 in that the modified diatomaceous earth filter aid was selected from that prepared in preparation example 5.
Fifth, performance test
Hydrogen-containing silicone oil was prepared by the methods in examples 1 to 3 and comparative examples 1 to 5, respectively, and the yield of the hydrogen-containing silicone oil was calculated; the filtration time required when the hydrogen-containing silicone oil was completely clear and transparent in examples 1 to 3 and S2 of comparative examples 1 to 5 was recorded to characterize the ease of separation of the catalyst from the silicone oil; the test was repeated by the methods of examples 1 to 3 and comparative examples 1 to 5, respectively, to test the viscosity change rate of the hydrogen-containing silicone oil when the catalyst was repeatedly used ten times; the test results are shown in table 1.
TABLE 1
The data in table 1 show that the yield of the hydrogen-containing silicone oil prepared by the method can reach more than 95%, and is superior to the catalytic efficiency of the traditional concentrated sulfuric acid catalyst with the same dosage, which indicates that the dosage of the modified activated clay catalyst used in the invention is lower on the premise that the catalyst and the traditional catalyst reach the same catalytic efficiency, thereby reducing the production cost; the post-treatment is mild and easy to operate, and the modified activated clay catalyst can be quickly separated by adopting the modified diatomite filter aid, so that the production process is simplified; in addition, the modified activated clay catalyst prepared by the method can be repeatedly used for many times, so that the production cost is further reduced.
The modified activated clay catalyst in comparative example 2 was a common activated clay provided by Henan Bokelong purification materials Co., Ltd.; compared with example 1, the yield of the hydrogen-containing silicone oil in comparative example 1 is obviously reduced, and the viscosity change rate of the hydrogen-containing silicone oil is obviously increased, which shows that the modified activated clay catalyst prepared by the invention has higher catalytic efficiency and can be reused more times compared with the traditional activated clay catalyst.
The modified activated clay catalyst of comparative example 3 was prepared from modified activated clay catalyst 4; compared with example 1, the yield of the hydrogen-containing silicone oil in the comparative example 3 is obviously reduced, and the viscosity change rate of the hydrogen-containing silicone oil is obviously increased, which shows that the addition of phosphotungstic acid in the modified activated clay catalyst prepared by the invention can obviously improve the catalytic efficiency of the hydrogen-containing silicone oil.
The modified diatomaceous earth filter aid of comparative example 4 was selected from that prepared in preparation example 4 of the modified diatomaceous earth filter aid; the modified diatomaceous earth filter aid of comparative example 5 was selected from the group consisting of those prepared in preparation example 5; compared with the example 1, the filtration time is obviously increased and the post-treatment difficulty is increased in the comparative examples 4 and 5, which shows that the adsorption filtration effect of the modified activated clay catalyst can be improved by adding the ferric chloride, the zeolite powder and the sodium ethylene diamine tetra methylene phosphonate into the preparation of the modified diatomite filter aid.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (5)
1. A preparation method of hydrogen-containing silicone oil is characterized by comprising the following steps: the method comprises the following steps: taking cyclosiloxane as a reaction monomer, adding a hydrogen end-capping agent, carrying out polymerization reaction under the action of a modified activated clay catalyst, adding a modified diatomite filter aid after the polymerization reaction is finished, carrying out circulating filtration until filtrate is clear and transparent, filtering the modified activated clay catalyst, and collecting clear and transparent liquid to obtain hydrogen-containing silicone oil;
the modified activated clay catalyst is prepared by the following method: taking 100 parts of water, adding 10-15 parts of phosphotungstic acid, and uniformly stirring to obtain a phosphotungstic acid solution; adding 30-40 parts of activated clay into the phosphotungstic acid solution, and stirring for 1-3 hours at the temperature of 80-90 ℃ to obtain activated clay suspension; thirdly, decompressing the activated clay suspension to-0.09 MPa, maintaining for 30-40min to obtain prefabricated activated clay, washing the prefabricated activated clay by water, and roasting at the temperature of 160-170 ℃ for 4-6h to obtain the modified activated clay catalyst;
the modified diatomite filter aid is prepared by the following method: (1) taking 100 parts of water, adding 10-15 parts of ferric chloride, and uniformly stirring to obtain a ferric chloride solution; (2) adding 50-60 parts of diatomite into the ferric chloride solution, and stirring for 1-2 hours at the temperature of 60-80 ℃ to obtain a diatomite suspension; (3) settling and filtering the diatomite suspension to obtain diatomite precipitate, washing the diatomite precipitate with water, roasting for 3-5h at the temperature of 130-140 ℃ to obtain modified diatomite, and granulating the modified diatomite to obtain a modified diatomite filter aid;
the granulation in step (3) is specifically performed as follows: adding sodium carbonate, kaolin, sodium bicarbonate, zeolite powder and sodium ethylene diamine tetra methylene phosphonate into the modified diatomite, adding an aqueous solution of polyvinyl alcohol while stirring, carrying out rolling granulation to obtain granules, and drying and roasting the granules to obtain the modified diatomite.
2. The method for preparing hydrogen-containing silicone oil according to claim 1, characterized in that: the hydrogen-terminated end-capping agent is 1,1,3, 3-tetramethyl dihydrodisiloxane; the cyclosiloxane is octamethylcyclotetrasiloxane.
3. The method for preparing hydrogen-containing silicone oil according to claim 1, characterized in that: the method specifically comprises the following steps:
s1, taking 29-75 parts by weight of hydrogen-terminated end-capping agent and 1900 parts by weight of cyclosiloxane, adding modified activated clay catalyst while stirring, heating to 80 ℃, and preserving heat for 8-12 hours to perform polymerization reaction;
and S2, after the polymerization reaction is finished, filtering the modified activated clay catalyst, and collecting clear and transparent liquid to obtain the hydrogen-containing silicone oil.
4. The method for preparing hydrogen-containing silicone oil according to claim 1, characterized in that: the stirring speed of the step II is 100-.
5. The method for preparing hydrogen-containing silicone oil according to claim 3, characterized in that: and (3) after the polymerization reaction in the S2, adding 10-15 parts of modified diatomite filter aid, and performing circulating filtration until the filtrate is clear and transparent.
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