CN113024808A - Preparation method of hydrogen-terminated silicone oil - Google Patents
Preparation method of hydrogen-terminated silicone oil Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 52
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 52
- 239000003054 catalyst Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 24
- UXJHQBVRZUANLK-UHFFFAOYSA-N azanylidyne(dichloro)-$l^{5}-phosphane Chemical compound ClP(Cl)#N UXJHQBVRZUANLK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 230000000694 effects Effects 0.000 claims abstract description 16
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 15
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 27
- -1 siloxane chain Chemical group 0.000 abstract description 15
- 229920001296 polysiloxane Polymers 0.000 abstract description 12
- 239000002253 acid Substances 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
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- 238000001816 cooling Methods 0.000 description 5
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
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- 238000009499 grossing Methods 0.000 description 1
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- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 230000002194 synthesizing effect Effects 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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)
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Silicon Polymers (AREA)
Abstract
The invention relates to a preparation method of hydrogen-terminated silicone oil, which adopts high-viscosity methyl silicone oil and hydrogen-containing double end sockets as raw materials to prepare the hydrogen-terminated silicone oil, under the action of a linear phosphonitrile chloride composite catalyst H, the catalyst has a degradation effect on siloxane chain segments in the methyl silicone oil chain segments to degrade macromolecular polysiloxane into a plurality of micromolecular polysiloxanes, meanwhile, the micromolecular polysiloxanes are subjected to polycondensation reaction rapidly, the hydrogen-containing double end sockets participate in the reaction in time and end-capping, the linear polysiloxanes are redistributed, and the high-activity hydrogen-terminated silicone oil is prepared. The method of the invention has no obvious cyclosiloxane generation, has little low-boiling-point substance content, and only generates extremely trace short-chain polysiloxane. The problems of low activity, low effective component, residual low-boiling-point substances and excessive ring bodies of the prepared target product in the traditional acid balance catalysis process are well solved, and the limit of international regulations such as reach and the like on the residual quantity of organosilicon ring body components such as D3, D4, D5 and the like in the product can be particularly met.
Description
Technical Field
The invention relates to the field of organosilicon softening agents, in particular to a preparation method of hydrogen-terminated silicone oil.
Background
In recent years, the organic silicon softening agent is developed extremely rapidly, and particularly, the terpolymer block silicone oil is an organic silicon softening finishing agent with a new structure which is developed most rapidly in recent decades. The ternary copolymerized silicone oil combines the polysiloxane chain segment, the polyether chain segment and the amino group on the same macromolecule. The polysiloxane chain segment mainly plays a role in straightening and smoothing, the polyether chain segment plays a role in self-emulsification and hydrophilicity, and the amino group mainly plays a role in softening. Compared with the traditional softening agent, the softening agent has more obvious linearity and excellent self-emulsifying property, can form stable emulsion by self-emulsifying in water, and has very outstanding overall comprehensive effect of softening finishing.
The hydrogen-terminated silicone oil is used as a basic raw material for synthesizing the block silicone oil, and the preparation method and the quality of the hydrogen-terminated silicone oil are one of the key factors for controlling the performance of the block silicone oil. The general synthesis of the hydrogen-terminated silicone oil can be obtained by telomerizing D4 (octamethylcyclotetrasiloxane) or DMC (dimethylcyclosiloxane mixture) and hydrogen-containing double-end-enclosure (tetramethyldihydro-disiloxane) as raw materials under the action of a catalyst. The selection of the catalyst is the key of the preparation. The difference of the catalyst not only relates to the difference of product performance, but also relates to the difficulty degree of production process control and the pressure in environmental protection.
At present, most manufacturers of hydrogen-terminated silicone oil prepared in the market adopt an acidic catalyst to carry out equilibrium reaction. In the market, the acidic catalyst mainly comprises concentrated sulfuric acid, activated clay, acidic resin, solid super acid and the like. The experimental results prove that: the hydrogen-containing silicone oil at the end of the preparation by acid balance catalysis has the best catalytic performance by concentrated sulfuric acid, but generates more solid wastes and is difficult to treat; the acidic resin can simplify the process flow, but has poor stability, and can cause the deactivation phenomenon of the catalyst to influence the performance of the product; activated clay is not conducive to the production operation. The invention provides a novel process for preparing hydrogen-terminated silicone oil with environmental protection and high efficiency, which breaks through the limit of the traditional acid catalyst and adopts a linear phosphonitrile chloride catalyst. The catalyst has excellent performance and extremely small using amount, greatly simplifies the synthesis process, and does not generate solid waste; the obtained target product contains hydrogen-containing silicone oil, has extremely low content of residual low-boiling-point substances and electrolytes, basically has no ring body residue, accords with the residue standard of international regulations, and is a new green, environment-friendly and efficient process.
Disclosure of Invention
The invention aims to provide a method for preparing hydrogen-terminated silicone oil which is green, environment-friendly, efficient and meets the international residue standard.
The invention relates to a preparation method of hydrogen-terminated silicone oil, which comprises the following steps:
s1, uniformly mixing high-viscosity methyl silicone oil and a hydrogen-containing double end socket;
s2, adding a linear phosphonitrile chloride composite catalyst into the uniformly mixed high-viscosity methyl silicone oil and the hydrogen-containing double end socket for catalytic reaction;
and S3, adding a terminator for reaction to deactivate the linear phosphonitrile chloride composite catalyst.
The invention adopts high-viscosity methyl silicone oil and hydrogen-containing double end sockets as raw materials to prepare hydrogen-containing end silicone oil, under the action of the linear phosphonitrile chloride composite catalyst H, the catalyst has a degradation effect on siloxane chain segments in the methyl silicone oil chain segments to degrade macromolecular polysiloxane into a plurality of micromolecular polysiloxanes, meanwhile, the micromolecular polysiloxanes are subjected to polycondensation reaction rapidly, the hydrogen-containing double end sockets participate in the reaction in time and end-seal, and the linear polysiloxanes are redistributed to prepare the high-activity hydrogen-containing end silicone oil. In the whole reaction process, no obvious cyclosiloxane is generated, the content of low-boiling-point substances is very little, and only a very trace amount of short-chain polysiloxane is generated. The problems of low activity, low effective component, residual low-boiling-point substances and excessive ring bodies of the prepared target product in the traditional acid balance catalysis process are well solved, and the limit of international regulations such as reach and the like on the residual quantity of organosilicon ring body components such as D3, D4, D5 and the like in the product can be particularly met.
Furthermore, in the S1, the weight ratio of the high-viscosity methyl silicone oil to the hydrogen-containing double end socket is 100: 0.4-100: 8.
The terminal hydrogen-containing silicone oil with different molecular weights can be prepared by adjusting the proportion of the methyl silicone oil and the hydrogen-containing double end socket, different industries can adjust according to the requirements of the industries, and the higher the methyl silicone oil input proportion is, the larger the molecular weight of the prepared terminal hydrogen-containing silicone oil is.
Further, in the step S2, the addition amount of the linear phosphonitrile chloride composite catalyst is one hundred thousandth to five hundred thousandth of the total weight of the high-viscosity methyl silicone oil and the hydrogen-containing double end socket.
The linear phosphonitrile chloride composite catalyst is used for carrying out catalytic reaction on high-viscosity methyl silicone oil and hydrogen-containing double end sockets, the performance is excellent, a very small amount of catalyst can achieve a good effect, the synthesis process is greatly simplified, and no solid waste is generated.
Further, the linear phosphonitrile chloride composite catalyst is diluted by inert liquid before being added.
Because the linear phosphonitrile chloride composite catalyst has excellent catalytic performance, a very small amount of catalyst can achieve a catalytic effect, and in order to achieve more uniform reaction, the catalyst is diluted and then added with high-viscosity methyl silicone oil and hydrogen-containing double-end-enclosure mixed liquid for catalytic reaction, so that the effect is better.
Further, in the step S2, the reaction temperature of the catalytic reaction is 60 to 70 ℃, and the reaction time is 0.5 to 2 hours.
In the catalytic reaction process, the high temperature is beneficial to reducing the viscosity of the methyl silicone oil and more beneficial to uniform mixing, but the hydrogen-containing double end socket has low boiling point and is easy to volatilize, so the temperature is not suitable to be too high, and the temperature is most suitable at 60-70 ℃.
Further, in the step S2, the mixed solution is stirred during the reaction, the stirring speed is 1000-2000 rpm in the first 0.5-1 hour, and the stirring speed is 150-400 rpm in the second 1-1.5 hour.
The stirring in the initial stage of the reaction is faster, and the stirring in the later stage can be slower, so that the reaction is more uniform.
Further, in the step S3, the weight ratio of the addition amount of the terminating agent to the addition amount of the linear phosphonitrile chloride composite catalyst in the step S2 is 1:1.1 to 1: 1.3.
Further, in the step S3, before the terminator is added, the temperature of the mixed solution of the high-viscosity methyl silicone oil and the hydrogen-containing double-end socket is raised to 80-100 ℃, and the reaction time is 10-30 minutes.
Further, in step S3, a dilution process is performed before the terminator is added.
The purpose of adding the terminating agent is to make the linear phosphonitrile chloride composite catalyst generate chemical reaction and lose activity. The more sufficient the reaction is, the better the effect is, the higher the quality of the obtained hydrogen-terminated silicone oil is, and the smaller the influence on the development of subsequent products is. The higher the temperature, the lower the viscosity, the more homogeneous the reaction and the faster the reaction rate. Because the addition amount of the terminating agent is also extremely small, the terminating agent can be fully mixed after dilution, and the linear phosphonitrile chloride composite catalyst is ensured to fully react and quickly lose activity.
Further, the method also includes step S4:
s4: and vacuumizing to remove low-boiling-point substances.
The hydrogen-terminated silicone oil prepared by the method has extremely low content of low-boiling-point substances, and the low-boiling-point substances can be further removed in a vacuumizing mode according to special requirements of different industries.
Compared with the prior art, the invention has the following advantages and effects:
1. the catalyst consumption is very small, and the cost is reduced;
2. the synthesis process is greatly simplified, and no solid waste is generated;
3. the prepared hydrogen-containing silicone oil has extremely low content of residual low-boiling residues and electrolytes, basically has no ring body residue, is more environment-friendly, and accords with the limit of international regulations on the residual quantity of organosilicon ring body components such as D3, D4, D5 and the like in products;
4. the preparation efficiency is higher.
Drawings
FIG. 1 is an infrared spectroscopic analysis chart of hydrogen-terminated silicone oil prepared by the method of the present invention.
Detailed Description
The present invention is described in further detail below by way of examples, which are illustrative of the present invention and are not intended to limit the present invention thereto.
Example (b):
the traditional process for preparing hydrogen-containing silicone oil: sequentially adding DMC or D4, hydrogen-containing double-end closure and concentrated sulfuric acid into a container, starting stirring, firstly heating to 30-35 ℃, and reacting for 6 hours under the condition of heat preservation. Then adding soda ash to neutralize and react for 1 hour to ensure that the pH value of the material is 6, and enabling the material to pass through a filtering device to remove generated solid wastes. Then the temperature is raised to 100 ℃ and 130 ℃, and the low-boiling-point substances are removed by vacuumizing. Finally, cooling and discharging to obtain the hydrogen-terminated silicone oil with the solid content of about 90 percent.
The new process for preparing hydrogen-containing silicone oil: the method comprises the steps of putting metered high-viscosity methyl silicone oil and hydrogen-containing double-end sockets into a container in sequence, fully mixing and stirring uniformly, adding a linear catalyst H, reacting at the temperature of 60-70 ℃ for 1-2H under the catalysis of the linear catalyst H, heating to 80-100 ℃, adding a terminator, and reacting for about 30min to inactivate the catalyst H in reactants. And then, according to the product requirements, determining whether to vacuumize to remove low-boiling-point substances or not to remove the low-boiling-point substances, and obtaining the high-solid-content hydrogen-terminated silicone oil with the content of more than 99 percent.
Experiment 1 (hydrogen-containing silicone oil-terminated 10K): in a flask equipped with a stirring device, 8 ten thousand viscosity methyl silicone oil: 200g and 3.0g of hydrogen-containing double end socket, fully mixing and stirring uniformly for 30min, then heating to 45 ℃, adding a linear catalyst H, carrying out heat preservation reaction for 1-2H at 60-70 ℃ under the catalysis of the linear catalyst H, then heating to 80-100 ℃, adding a terminator, and reacting for about 30min to inactivate the catalyst H in the reactant. Then cooling to 40-50 ℃, discharging to obtain the hydrogen-terminated silicone oil with high solid content of more than 99%.
Sampling to test the viscosity of the target product: 203mpa.s hydrogen content: 0.020%, solid content: 99.5 percent
Experiment 2: (hydrogen-terminated silicone oil 8K): in a flask equipped with a stirring device, 8 ten thousand viscosity methyl silicone oil: 200g and 3.95g of hydrogen-containing double end socket, fully mixing and stirring uniformly for 30min, then heating to 45 ℃, adding a linear catalyst H, carrying out heat preservation reaction for 1-2H at 60-70 ℃ under the catalysis of the linear catalyst H, then heating to 80-100 ℃, adding a terminator, and reacting for about 30min to inactivate the catalyst H in the reactant. Then cooling to 40-50 ℃, discharging to obtain the hydrogen-terminated silicone oil with high solid content of more than 99%.
Sampling to test the viscosity of the target product: 138mpa.s hydrogen content: 0.025%, solid content: 99.4 percent
Experiment 3: (hydrogen-terminated silicone oil 13K): in a flask equipped with a stirring device, 8 ten thousand viscosity methyl silicone oil: 200g of hydrogen-containing double-end socket 2.36g, fully mixing and stirring uniformly for 30min, then heating to 45 ℃, adding a linear catalyst H, carrying out heat preservation reaction for 1-2H at 60-70 ℃ under the catalysis of the linear catalyst H, then heating to 80-100 ℃, adding a terminator, and reacting for about 30min to inactivate the catalyst H in the reactant. Then cooling to 40-50 ℃, discharging to obtain the hydrogen-terminated silicone oil with high solid content of more than 99%.
Sampling to test the viscosity of the target product: 357mpa.s hydrogen content: 0.015%, solid content: 99.5 percent
The three key data of the viscosity, the hydrogen content and the solid content of the tested product are all in a reasonable range, compared with the traditional preparation method, the viscosity is slightly increased, the hydrogen content is kept consistent, and the solid content is increased to more than 99 percent, the data show that the hydrogen-containing silicone oil prepared by the process has higher effective components, and the residual low-boiling-point substances, electrolytes and organic silicon ring bodies are extremely low, so that the accuracy and the reliability of the process are further explained.
Analysis of the above experiment can yield fig. 1.
As shown in FIG. 1, the broad absorption peak at 3700cm-1 on the infrared spectrogram is the OH absorption peak; an absorption peak of C-H appears at 2962 cm-1; a si-H bending vibration absorption peak appears at 2127 cm-1; 1412cm-1 is C-H bending vibration; 1259cm-1 is the characteristic absorption peak of Si-CH 3; 1093cm-1,1019cm-1 is the characteristic absorption peak of Si-O-Si; 799cm-1 is a characteristic absorption peak of Si-CH3 and Si-CH 2-; wherein 1093cm-1,1019cm-1 is the overlapped absorption peak of C-O-C; an absorption peak of C ═ O appears at 1640 cm-1; while a broad and short peak at 3700cm-1 also indicates hydroxyl termination.
It can be seen that the structure contains silicon-hydrogen, polysiloxane, methyl and other structures, and the main product is hydrogen-terminated silicone oil, but inevitably contains a certain amount of dimethyl silicone oil and single-terminated hydrogen silicone oil.
The high-viscosity methyl silicone oil is used for synthesis, so that the high content of the terminal hydrogen-containing silicone oil in the product can be ensured.
The production process of the hydrogen-terminated silicone oil prepared by the new process is used for producing the subsequent block silicone oil, the production process of the hydrogen-terminated silicone oil prepared by the new process and the production process of the hydrogen-terminated silicone oil prepared by the traditional process for producing the subsequent block silicone oil can adopt the same process, but in the reaction process, the hydrogen-terminated silicone oil and the traditional process show certain performance difference from the reaction temperature rise speed and the reaction temperature rise range, so that the performance of the block silicone oil produced by the hydrogen-terminated silicone oil and the traditional process has certain difference.
The hydrogen-terminated silicone oil prepared by the novel process is used for the subsequent block silicone oil synthesis process:
putting the metered hydrogen-terminated silicone oil 10K (with the molecular weight of 10000), allyl epoxy polyoxyethylene ether and butyl ether into a container with a thermometer and a stirrer, stirring and heating to 45 ℃, adding a chloroplatinic acid complex catalyst, gradually heating to 90-95 ℃, and carrying out heat preservation reaction for 4-6 h; a pale yellow transparent liquid (epoxy terminated polyether silicone oil) was obtained. Then adding a metered amount of polyether amine ED900, and reacting for 6-8h at the temperature of 93-95 ℃ in a heat preservation manner; and (4) after heat preservation, cooling to 40-50 ℃, and adding a proper amount of glacial acetic acid to obtain the faint yellow viscous block silicone oil crude oil.
The hydrogen-terminated silicone oil prepared by the traditional old process is used for the subsequent block silicone oil synthesis process, after a catalyst is added at 45 ℃, the hydrosilylation reaction of the system is slow, the temperature rises slowly and can rise to 90 ℃ after 1 hour, and the heat preservation reaction lasts for 2-3 hours to obtain light yellow transparent liquid.
The hydrogen-terminated silicone oil prepared by the process is used for the subsequent block silicone oil synthesis process, under the same conditions, after the catalyst is added, the system temperature rises quickly, can rise to 90 ℃ in about 45min, and is subjected to heat preservation reaction for 1.5-2h, so that light yellow transparent end epoxy polyether silicone oil can be obtained; and then ED900 is added for aminolysis ring-opening reaction, and finally the block silicone oil crude oil is obtained. The crude oil prepared by the new process is light yellow and transparent, and the transparency is far higher than that of the traditional process. Therefore, the hydrogen-terminated silicone oil prepared by the new process has stronger activity and higher retention rate of silicon-hydrogen bonds, and is easier to carry out hydrosilylation reaction and subsequent reaction. When the fabric is applied to fabrics, the soft hand feeling is similar, and the smooth hand feeling and the fineness are improved, so that the comprehensive hand feeling is superior to that of the traditional process. The analysis reason is that in the hydrogen-terminated silicone oil prepared by the new process, the residual low-boiling-point substances, electrolytes and organic silicon ring bodies are extremely low, the reaction activity is strong, the addition of silicon hydrogen is sufficient, and the effective components of the obtained block silicone oil are high, so that the emulsion stability is good, and the comprehensive hand feeling is improved.
In addition, it should be noted that the specific embodiments described in the present specification may be different in terms of the parts, the shapes of the components, the process steps, the names of the methods, and the like. All equivalent or simple changes of the structure, the characteristics and the principle of the invention which are described in the patent conception of the invention are included in the protection scope of the patent of the invention. Various modifications, additions and substitutions for the specific embodiments described may be made by those skilled in the art without departing from the scope of the invention as defined in the accompanying claims.
Claims (10)
1. The preparation method of the hydrogen-terminated silicone oil is characterized by comprising the following steps:
s1, uniformly mixing high-viscosity methyl silicone oil and a hydrogen-containing double end socket;
s2, adding a linear phosphonitrile chloride composite catalyst into the uniformly mixed high-viscosity methyl silicone oil and the hydrogen-containing double end socket for catalytic reaction;
and S3, adding a terminator to react so that the linear phosphonitrile chloride composite catalyst loses activity.
2. The method for preparing terminal hydrogen-containing silicone oil according to claim 1, wherein in S1, the weight ratio of the high-viscosity methyl silicone oil to the hydrogen-containing double end socket is 100:0.4 to 100: 8.
3. The method for preparing terminal hydrogen-containing silicone oil according to claim 1, wherein in step S2, the amount of the linear phosphonitrile chloride composite catalyst added is one hundred thousandth to five hundred thousandth of the total weight of the high-viscosity methyl silicone oil and the hydrogen-containing double end socket.
4. The method for preparing terminal hydrogen-containing silicone oil according to claim 3, wherein the linear phosphonitrile chloride composite catalyst is diluted with an inert liquid before being added.
5. The method for preparing terminal hydrogen-containing silicone oil according to claim 3, wherein in step S2, the reaction temperature of the catalytic reaction is 60-70 ℃ and the reaction time is 0.5-2 hours.
6. The method as claimed in claim 5, wherein in step S2, the mixture is stirred during the reaction, the stirring speed is 1000-2000 rpm for the first 0.5-1 hour, and the stirring speed is 150-400 rpm for the second 1-1.5 hours.
7. The method for preparing terminal hydrogen-containing silicone oil according to claim 1, wherein the weight ratio of the addition amount of the terminating agent in step S3 to the addition amount of the linear phosphonitrile chloride composite catalyst in step S2 is 1:1.1 to 1: 1.3.
8. The method for preparing terminal hydrogen-containing silicone oil according to claim 7, wherein in step S3, the temperature of the mixed solution of high-viscosity methyl silicone oil and hydrogen-containing double end enclosure is raised to 80-100 ℃ for 10-30 minutes before the terminator is added.
9. The method for preparing terminal hydrogen-containing silicone oil according to claim 8, wherein in step S3, the terminating agent is diluted before being added.
10. The method for preparing hydrogen-terminated silicone oil according to any one of claims 1 to 9, further comprising step S4:
s4: and vacuumizing to remove low-boiling-point substances.
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| CN113896893A (en) * | 2021-10-11 | 2022-01-07 | 湖北兴瑞硅材料有限公司 | Preparation method of high-conversion low-cycle-content simethicone |
| CN115676785A (en) * | 2022-09-09 | 2023-02-03 | 新纳奇材料科技江苏有限公司 | Preparation method of phosphonitrile chloride catalyst and application of phosphonitrile chloride catalyst in preparation of hydrogen-containing silicone oil |
| CN115772265A (en) * | 2023-02-10 | 2023-03-10 | 山东东岳有机硅材料股份有限公司 | Vinyl fluorine-containing polysiloxane and preparation method thereof |
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