CN103788377A - Production process for continuously producing high-hydrogen-content silicone oil - Google Patents
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Abstract
The invention discloses a production process for continuously producing high-hydrogen-content silicone oil. The production process comprises the following steps: performing hydrolysis reaction on raw materials including trimethylchlorosilane, methyldichlorosilane, diluted hydrochloric acid and low molecule, which are in proportion; separating an oil acid mixture obtained by the hydrolysis reaction, feeding a hydrolysate at the upper layer into a washing system for deacidification, feeding dilute acid at the lower layer into a hydrolysis reaction system for recycling; after the washed hydrolysate is dehydrated, feeding the dehydrated hydrolysate into a fixed bed reaction system filled with a catalyst, and performing telomeric reaction on hydrogen-containing silicone oil; performing decontaminating, low molecule removal and refining on the hydrogen-containing silicone oil subjected to the telomeric reaction to obtain the hydrogen-containing silicone oil of which the hydrogen content is 1.56-1.60wt%. The production process for the high-hydrogen-content silicone oil, provided by the invention, has the advantages of low energy consumption, high yield, low production cost, high product hydrogen content and the like.
Description
Technical field
The present invention relates to a kind of production method of field of fine chemical, especially relate to a kind of serialization and prepare high containing hydrogen silicone oil production technique.
Background technology
The high containing hydrogen silicone oil of methyl is a kind of water white oily liquids, and viscosity is generally 10～200 mPaS, is one of product important in silicone oil kind.In its siloxane main chain, contain reactive group hydrogen, active high, can react with many active groups.Its distinguishing feature is good water-proof effect.Can crosslinked at low temperature film forming, form waterproof layer on the surface of material, be widely used in the water-resisting agent of the industries such as fabric, glass, pottery, paper, leather, metal, building materials and silicon rubber anti-yellowing dose, linking agent, silicon rubber printing ink reducer etc., effect is excellent.
The synthetic of the high containing hydrogen silicone oil of methyl mainly telomerized or formed by methylhydrocyclosiloxane ring opening copolymer by the hydrolysis of methyl hydrogen dichlorosilane monomer, and preparation process generally comprises non-solvent method and solvent method two classes.Solvent method removes because the solvent using in this technique need to consume a lot of energy, and solvent itself also can exist safety problem, and in addition, residual quality on the product impact of solvent in product is very large.Thereby advance in the whole world under the background of Green Chemistry, solventless method is gone on the arena of history gradually.
The shortcomings such as the solventless method explained hereafter containing hydrogen silicone oil adopting mostly at present is batch process, and its production cost is high, hydrogen content is low, production efficiency is low have hindered its development.Patent CN102516545A has announced a kind of method of serialization production containing hydrogen silicone oil, but in this technique, need to use the vitriol oil to telomerize, utilize alkali to neutralize, and need to consume a large amount of water and wash, in the process of washing, also easily produce emulsification simultaneously and make the yield of containing hydrogen silicone oil very low; Because need to wash many times, in water washing process, also easily cause emulsification to make profit be difficult to separate.In addition, only utilize water to be hydrolyzed and make to produce the dilute hydrochloric acid that a large amount of concentration is very low, the desorption of these hydrochloric acid need to consume a large amount of energy.Thereby need to containing hydrogen silicone oil production technique be further improved and be innovated.
Summary of the invention
The object of this invention is to provide a kind of serialization and produce the production technique of high containing hydrogen silicone oil.
What the present invention solved is that the solvent itself existing during existing solvent process is produced exists pollution or side effect, in product there is restriction in the residual utilization to product of solvent, and production cost that non-solvent method explained hereafter containing hydrogen silicone oil exists is high, yield is low, containing hydrogen number problem on the low side.
Technical scheme of the present invention is: the production technique of high containing hydrogen silicone oil is produced in a kind of serialization, and described production technique comprises the following steps:
Step 1: trimethylchlorosilane, methyl hydrogen dichlorosilane, dilute hydrochloric acid, low molecule are joined in hydrolysis circulating reaction system by a certain percentage, and mean residence time is 20～100min, and temperature of reaction is 5 ℃～30 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:10～50, and described trimethylchlorosilane and the chlorosilane mixture of methyl hydrogen dichlorosilane composition and the mass ratio of dilute hydrochloric acid are 1:20～100;
Step 2: the oleic acid mixture obtaining through hydrolysis reaction enters in oleic acid separation system and separates, and after separation, upper strata obtains hydrolyzate, and lower floor obtains diluted acid; The residence time of described upper strata hydrolyzate in oleic acid separation system is 50～150min; Described lower floor diluted acid enters the further recycle of hydrolysising reacting system in described step 1; Described upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate, enters and in dewatering system, carry out processed after described hydrolyzate deacidification;
Step 3: enter in the fixed bed reaction system that catalyzer is housed and carry out containing hydrogen silicone oil telomerization through the hydrolyzate of processed, the temperature of described telomerization is controlled at 20～60 ℃, and the time of telomerizing is controlled at 2～6h; The containing hydrogen silicone oil obtaining through telomerization enters in filtering system and removes impurity, enters de-low molecule device and deviates from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in the hydrolysis circulating reaction system of described step 1; The described de-low time is 5min～60min, and temperature is controlled at 100 ℃～120 ℃; Containing hydrogen silicone oil after de-low enters in containing hydrogen silicone oil refining system to be refined, and can obtain high hydrogeneous containing hydrogen silicone oil; The hydrogen content of the described containing hydrogen silicone oil obtaining is 1.56～1.60wt%.
Hydrolysis circulating reaction system in described step 1 is made up of venturi mixer, static mixer, interchanger, hydrolysis recycle pump.
The dilute hydrochloric acid concentration that in described step 1, hydrolysis reaction uses is 1～5wt%.
In described step 2, water wash system is made up of coalescer and oil-water decanter.
Catalyzer in described step 3 is one or both the mixture in acidic white earth, strong-acid ion exchange resin.
De-low molecule device in described step 2 is the combination of any in rotating scraper evaporator, falling-film evaporator, decompression stirring tank, vaporizer or two kinds.
Treating process in described step 2 comprises that employing charcoal absorption and strainer filter.
Further, in described step 2, the material of coalescer filter core is the one in glass fibre, trevira, steel fiber, sintering felt, polypropylene fiber, polyster fibre.
Further, the material of described step 2 middle filtrator filter core comprises urethane and trevira.
The beneficial effect that the present invention produces is: the present invention adopts the hydrolysis recycle system that the raw material hydrolysis of producing high containing hydrogen silicone oil can be carried out in inferior quality concentration hydrochloric acid soln; Adopt static mixer, these static equipments of venturi-type eductors that the energy consumption of hydrolytic process is reduced greatly, adopt in water wash system, add coalescer carry out oily water separation make washing number of times reduce, the efficiency of washing improves greatly, avoid the emulsion in water washing process, improve the yield of high containing hydrogen silicone oil, thereby high containing hydrogen silicone oil production cost prepared by this technique is reduced greatly; Meanwhile, the hydrolysis recycle system has shortened the residence time of high containing hydrogen silicone oil in concentrated acid, and the hydrogen content of containing hydrogen silicone oil prepared by this technique is remained between 1.56～1.60wt%.
Accompanying drawing explanation
Fig. 1 is production technological process of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) dilute hydrochloric acid that is 1wt% trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, low molecule join in hydrolysis circulating reaction system in proportion, mean residence time 20min, and temperature is 8 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:10, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 1wt% are 1:30;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata is hydrolyzate, the dilute hydrochloric acid that lower floor is 16wt%; Described lower floor diluted acid enters hydrolysising reacting system and carries out recycle; The residence time of described upper strata hydrolyzate in oleic acid separation system is 50min; Described upper strata hydrolyzate enters water wash system and washes, and removes the acid in hydrolyzate; Upper strata hydrolyzate enters in dewatering system and dewaters;
3) hydrolyzate of process dehydration enters to be equipped with in the fixed bed reaction system that catalyzer is acidic white earth and carries out containing hydrogen silicone oil telomerization, telomerizes temperature and is controlled at 50 ℃, and the time of telomerizing is controlled at 4h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out, described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, the de-low time is 20min, temperature is controlled at 120 ℃, containing hydrogen silicone oil after de-low enters in containing hydrogen silicone oil refining system to be refined, and can obtain high hydrogeneous containing hydrogen silicone oil.The viscosity of the containing hydrogen silicone oil product of preparation is 18(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.59wt%.
Embodiment 2
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) dilute hydrochloric acid that is 3wt% trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, low molecule join in hydrolysis circulating reaction system in proportion, mean residence time 40min, and temperature is 12 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:20, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 3wt% are 1:40;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 20wt%; Lower floor's diluted acid enters hydrolysising reacting system recycle; The residence time of upper strata hydrolyzate in oleic acid separation system is 80min, and upper strata hydrolyzate enters in water wash system and removes the acid in hydrolyzate, then enters in dewatering system and dewaters;
3) hydrolyzate of process dehydration enters to be equipped with in the fixed bed reaction system that catalyzer is acidic white earth and carries out containing hydrogen silicone oil telomerization, telomerizes temperature and is controlled at 60 ℃, and the time of telomerizing is controlled at 3h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out, described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 50min, temperature is controlled at 100 ℃, and de-containing hydrogen silicone oil after low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 21(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.58 wt %.
Embodiment 3
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) dilute hydrochloric acid that is 5wt% trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, low molecule join in hydrolysis circulating reaction system in proportion, mean residence time 30min, and temperature is 20 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:30, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 5wt% are 1:80;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 22wt%, and wherein the residence time of hydrolyzate in oleic acid separation system is 100min; Upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate; Lower floor's diluted acid enters hydrolysising reacting system recycle, and upper strata hydrolyzate enters in dewatering system and dewaters;
3) hydrolyzate of process dehydration enters to be equipped with in the fixed bed reaction system that catalyzer is acidic white earth and carries out containing hydrogen silicone oil telomerization, telomerizes temperature and is controlled at 30 ℃, and the time of telomerizing is controlled at 6h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 30min, temperature is controlled at 120 ℃, the containing hydrogen silicone oil after de-low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 20(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.59wt%.
Embodiment 4
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) be that the dilute hydrochloric acid of 5wt %, low molecule join in hydrolysis circulating reaction system in proportion trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, mean residence time 90min, temperature is 10 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:45, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 5wt% are 1:90;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 21wt%, and wherein the residence time of hydrolyzate in oleic acid separation system is 120min; Upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate; Lower floor's diluted acid enters hydrolysising reacting system recycle, and upper strata hydrolyzate enters in dewatering system and dewaters;
3) hydrolyzate of process dehydration enters to be equipped with in the fixed bed reaction system that catalyzer is strong-acid ion exchange resin and carries out containing hydrogen silicone oil telomerization, telomerizes temperature and is controlled at 60 ℃, and the time of telomerizing is controlled at 3h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 60min, temperature is controlled at 100 ℃, the containing hydrogen silicone oil after de-low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 22(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.57 wt %.
Embodiment 5
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) be that the dilute hydrochloric acid of 4wt %, low molecule join in hydrolysis circulating reaction system in proportion trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, mean residence time 90min, temperature is 10 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:50, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 4wt% are 1:60;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 25wt%, and wherein the residence time of hydrolyzate in oleic acid separation system is 100min; Upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate; Lower floor's diluted acid enters hydrolysising reacting system recycle, and upper strata hydrolyzate enters in dewatering system and dewaters;
3) hydrolyzate of process dehydration enters to be equipped with in the fixed bed reaction system that catalyzer is strong-acid ion exchange resin and carries out containing hydrogen silicone oil telomerization, telomerizes temperature and is controlled at 30 ℃, and the time of telomerizing is controlled at 6h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 60min, temperature is controlled at 105 ℃, the containing hydrogen silicone oil after de-low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 19(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.59wt%.
Embodiment 6
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) be that the dilute hydrochloric acid of 3wt %, low molecule join in hydrolysis circulating reaction system in proportion trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, mean residence time 90min, temperature is 6 ℃; The quality of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:40, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 3wt% are 1:75;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 20wt%, and wherein the residence time of hydrolyzate in oleic acid separation system is 120min; Upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate; Lower floor's diluted acid enters hydrolysising reacting system recycle, and upper strata hydrolyzate enters in dewatering system and dewaters;
3) hydrolyzate of process dehydration enters to be equipped with in the fixed bed reaction system that catalyzer is strong-acid ion exchange resin and carries out containing hydrogen silicone oil telomerization, telomerizes temperature and is controlled at 40 ℃, and the time of telomerizing is controlled at 5h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 60min, temperature is controlled at 110 ℃, the containing hydrogen silicone oil after de-low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 18(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.60 wt %.
Embodiment 7
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) be that the dilute hydrochloric acid of 3wt %, low molecule join in hydrolysis circulating reaction system in proportion trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, mean residence time 90min, temperature is 15 ℃; The quality of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:40, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 3wt% are 1:70;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 20wt%, and wherein the residence time of hydrolyzate in oleic acid separation system is 125min; Upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate; Lower floor's diluted acid enters hydrolysising reacting system recycle, and upper strata hydrolyzate enters in dewatering system and dewaters;
3) enter in the fixed bed reaction system that acidic white earth and strong-acid ion exchange resin mixed catalyst are housed and carry out containing hydrogen silicone oil telomerization through the hydrolyzate of dehydration, telomerize temperature and be controlled at 40 ℃, the time of telomerizing is controlled at 6h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 50min, temperature is controlled at 110 ℃, the containing hydrogen silicone oil after de-low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 18(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.60 wt %.
Embodiment 8
The production technique that high containing hydrogen silicone oil is produced in a kind of serialization comprises the following steps:
1) be that the dilute hydrochloric acid of 3wt %, low molecule join in hydrolysis circulating reaction system in proportion trimethylchlorosilane, methyl hydrogen dichlorosilane, concentration, mean residence time 100min, temperature is 12 ℃; The quality of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:45, and the chlorosilane mixture of trimethylchlorosilane and methyl hydrogen dichlorosilane composition and the mass ratio of the dilute hydrochloric acid that concentration is 3wt% are 1:80;
2) the oleic acid mixture obtaining through hydrolysis reaction separates in oleic acid separation system, and upper strata obtains hydrolyzate, and lower floor obtains the dilute hydrochloric acid of 20wt%, and wherein the residence time of hydrolyzate in oleic acid separation system is 120min; Upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate; Lower floor's diluted acid enters hydrolysising reacting system recycle, and upper strata hydrolyzate enters in dewatering system and dewaters;
3) enter in the fixed bed reaction system that acidic white earth and strong-acid ion exchange resin mixed catalyst are housed and carry out containing hydrogen silicone oil telomerization through the hydrolyzate of dehydration, telomerize temperature and be controlled at 35 ℃, the time of telomerizing is controlled at 6h; Enter and in filtering system, remove impurity through the containing hydrogen silicone oil of telomerization; Enter de-low molecule device and deviate from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in hydrolysis circulating reaction system, de-low time 60min, temperature is controlled at 120 ℃, the containing hydrogen silicone oil after de-low enters and refiningly in containing hydrogen silicone oil refining system can obtain high hydrogeneous containing hydrogen silicone oil.The containing hydrogen silicone oil product of preparation: viscosity is 18(25 ℃, mm
2/ s), pH value is 7.0, hydrogen content is 1.60 wt %.
Claims (9)
1. a production technique for high containing hydrogen silicone oil is produced in serialization, it is characterized in that described production technique comprises the following steps:
Step 1: trimethylchlorosilane, methyl hydrogen dichlorosilane, dilute hydrochloric acid, low molecule are joined in hydrolysis circulating reaction system by a certain percentage, and mean residence time is 20～100min, and temperature of reaction is 5 ℃～30 ℃; The mass ratio of described trimethylchlorosilane and methyl hydrogen dichlorosilane is 1:10～50, and described trimethylchlorosilane and the chlorosilane mixture of methyl hydrogen dichlorosilane composition and the mass ratio of dilute hydrochloric acid are 1:20～100;
Step 2: the oleic acid mixture obtaining through hydrolysis reaction enters in oleic acid separation system and separates, and after separation, upper strata obtains hydrolyzate, and lower floor obtains diluted acid; The residence time of described upper strata hydrolyzate in oleic acid separation system is 50～150min; Described lower floor diluted acid enters the further recycle of hydrolysising reacting system in described step 1; Described upper strata hydrolyzate enters and in water wash system, removes the acid in hydrolyzate, enters and in dewatering system, carry out processed after described hydrolyzate deacidification;
Step 3: enter in the fixed bed reaction system that catalyzer is housed and carry out containing hydrogen silicone oil telomerization through the hydrolyzate of processed, the temperature of described telomerization is controlled at 20～60 ℃, and the time of telomerizing is controlled at 2～6h; The containing hydrogen silicone oil obtaining through telomerization enters in filtering system and removes impurity, enters de-low molecule device and deviates from low molecule from strainer containing hydrogen silicone oil out; Described deviate from low molecule enter further recycle in the hydrolysis circulating reaction system of described step 1; The described de-low time is 5min～60min, and temperature is controlled at 100 ℃～120 ℃; Containing hydrogen silicone oil after de-low enters in containing hydrogen silicone oil refining system to be refined, and can obtain high hydrogeneous containing hydrogen silicone oil; The hydrogen content of the described containing hydrogen silicone oil obtaining is 1.56～1.60wt%.
2. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 1, is characterized in that the hydrolysis circulating reaction system in described step 1 is made up of venturi mixer, static mixer, interchanger, hydrolysis recycle pump.
3. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 1, is characterized in that the dilute hydrochloric acid concentration that in described step 1, hydrolysis reaction uses is 1～5wt%.
4. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 1, is characterized in that in described step 2, water wash system is made up of coalescer and oil-water decanter.
5. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 1, is characterized in that catalyzer in described step 3 is one or both the mixture in acidic white earth, strong-acid ion exchange resin.
6. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 1, is characterized in that de-low molecule device in described step 2 is the combination of any in rotating scraper evaporator, falling-film evaporator, decompression stirring tank, vaporizer or two kinds.
7. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 1, is characterized in that the treating process in described step 2 comprises that employing charcoal absorption and strainer filter.
8. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 4, the material that it is characterized in that described coalescer filter core is the one in glass fibre, trevira, steel fiber, sintering felt, polypropylene fiber, polyster fibre.
9. the production technique that high containing hydrogen silicone oil is produced in a kind of serialization according to claim 7, is characterized in that the material of described filter element comprises urethane and trevira.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104140531A (en) * | 2014-07-30 | 2014-11-12 | 成都博达爱福科技有限公司 | Solvent-free continuous preparation method suitable for methyl hydrogen silicone oil |
| CN104140532A (en) * | 2014-07-30 | 2014-11-12 | 成都博达爱福科技有限公司 | Solvent-free process method for continuously producing methyl hydrogen silicone oil |
| CN104710618A (en) * | 2015-03-16 | 2015-06-17 | 南京博明科技有限责任公司 | Production technology for continuously producing high-hydrogen silicone oil |
| CN105732986A (en) * | 2016-01-27 | 2016-07-06 | 江西品汉新材料有限公司 | Technology for preparing methyl hydrogen silicone oil |
| CN107417920A (en) * | 2017-09-01 | 2017-12-01 | 合盛硅业股份有限公司 | A kind of system and method for producing high containing hydrogen silicone oil |
| CN111004394A (en) * | 2019-12-24 | 2020-04-14 | 唐山三友硅业有限责任公司 | Method for preparing high hydrogen-containing silicone oil by low molecule of high hydrogen-containing silicone oil and combination of acid and medium oil |
| CN111170272A (en) * | 2020-01-07 | 2020-05-19 | 浙江新安化工集团股份有限公司 | Hydrogen storage material, application thereof and energy conversion device |
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| CN102516545A (en) * | 2011-11-11 | 2012-06-27 | 江苏创基新材料有限公司 | Method for continuously producing hydrogen-containing silicon oil |
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| CN102516545A (en) * | 2011-11-11 | 2012-06-27 | 江苏创基新材料有限公司 | Method for continuously producing hydrogen-containing silicon oil |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140531A (en) * | 2014-07-30 | 2014-11-12 | 成都博达爱福科技有限公司 | Solvent-free continuous preparation method suitable for methyl hydrogen silicone oil |
| CN104140532A (en) * | 2014-07-30 | 2014-11-12 | 成都博达爱福科技有限公司 | Solvent-free process method for continuously producing methyl hydrogen silicone oil |
| CN104710618A (en) * | 2015-03-16 | 2015-06-17 | 南京博明科技有限责任公司 | Production technology for continuously producing high-hydrogen silicone oil |
| CN105732986A (en) * | 2016-01-27 | 2016-07-06 | 江西品汉新材料有限公司 | Technology for preparing methyl hydrogen silicone oil |
| CN105732986B (en) * | 2016-01-27 | 2018-10-19 | 江西品汉新材料有限公司 | A kind of technique preparing Methyl Hydrogen Polysiloxane Fluid |
| CN107417920A (en) * | 2017-09-01 | 2017-12-01 | 合盛硅业股份有限公司 | A kind of system and method for producing high containing hydrogen silicone oil |
| CN111004394A (en) * | 2019-12-24 | 2020-04-14 | 唐山三友硅业有限责任公司 | Method for preparing high hydrogen-containing silicone oil by low molecule of high hydrogen-containing silicone oil and combination of acid and medium oil |
| CN111170272A (en) * | 2020-01-07 | 2020-05-19 | 浙江新安化工集团股份有限公司 | Hydrogen storage material, application thereof and energy conversion device |
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