CN103788377B - A kind of production technology of continuous prodution height containing hydrogen silicone oil - Google Patents
A kind of production technology of continuous prodution height containing hydrogen silicone oil Download PDFInfo
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Abstract
The invention discloses the production technology of a kind of continuous prodution height containing hydrogen silicone oil, its processing step is: be hydrolyzed by a certain percentage reaction with trim,ethylchlorosilane, methyl hydrogen dichlorosilane, dilute hydrochloric acid, low molecule for raw material, after the oleic acid mixture separation that hydrolysis obtains, upper strata hydrolysate enters in water wash system and deacidifies, and the diluted acid that lower floor obtains enters hydrolysising reacting system and recycles；After hydrolysate after washing is dehydrated, enter equipped with catalyst fixed bed response system carries out containing hydrogen silicone oil telomerisation；Through telomerisation containing hydrogen silicone oil by remove impurity, de-low, refined after can obtain the containing hydrogen silicone oil that hydrogen content is 1.56～1.60wt%.The high containing hydrogen silicone oil production technology that the present invention provides has the advantages such as energy consumption is low, yield is high, production cost is low, product hydrogen content is high.
Description
Technical field
The present invention relates to the production method of a kind of field of fine chemical, especially relate to a kind of serialization and prepare high containing hydrogen silicone oil production technology.
Background technology
Methyl height containing hydrogen silicone oil is a kind of water white oily liquids, and viscosity is generally 10～200 mPa S, is one of product important in silicone oil kind.Containing reactive group hydrogen in its siloxane main chain, activity is high, can react with many active groups.Its distinguishing feature is good water-proof effect.Can form waterproof layer on the surface of material with crosslinked at low temperature film forming, be widely used in the waterproofing agent of the industries such as fabric, glass, pottery, paper, leather, metal, building materials and anti-yellowing dose of silicone rubber, cross-linking agent, silicone rubber printing ink reducer etc., effect is favourable.
The synthesis of methyl height containing hydrogen silicone oil is mainly telomerized by the hydrolysis of methyl hydrogen dichlorosilane monomer or is formed by methylhydrocyclosiloxane ring opening copolymer, and preparation process generally comprises non-solvent method and solvent method two class.Solvent method is removed owing to the solvent used in this technique needs to consume a lot of energy, and solvent itself also can exist safety problem, additionally, the residual that solvent is in the product is the biggest to the qualitative effects of product.Thus under the whole world advances the background of Green Chemistry, solventless method gradually goes on the arena of history.
The shortcomings such as the solventless method technique used at present produces containing hydrogen silicone oil and mostly is batch process, and its production cost is high, hydrogen content is low, production efficiency is low hinder its development.Patent CN102516545A
A kind of method disclosing continuous prodution containing hydrogen silicone oil, but this technique needs use concentrated sulphuric acid to telomerize, utilize alkali to be neutralized, and need to consume substantial amounts of water and wash, be also easy to produce emulsifying simultaneously during washing and make the yield of containing hydrogen silicone oil the lowest；Since it is desired that wash many times, water-washing process is also easy to cause emulsifying to make profit be difficult to separate.Additionally, be hydrolyzed the dilute hydrochloric acid the lowest so that producing a large amount of concentration just with water, the desorption of these hydrochloric acid needs to consume substantial amounts of energy.So that containing hydrogen silicone oil production technology is further improved and innovates.
Summary of the invention
It is an object of the invention to provide the production technology of a kind of continuous prodution height containing hydrogen silicone oil.
What the present invention solved is that present in existing solvent process produces, solvent itself exists pollution or side effect, in product there is restriction to the utilization of product in the residual of solvent, and non-solvent method technique produces that the production cost that containing hydrogen silicone oil exists is high, yield is low, containing hydrogen number problem on the low side.
The technical scheme is that the production technology of a kind of continuous prodution height containing hydrogen silicone oil, described production technology comprises the following steps:
Step 1: be that raw material joins in hydrolysis circulating reaction system by a certain percentage by trim,ethylchlorosilane, methyl hydrogen dichlorosilane, the low molecule of dilute hydrochloric acid, mean residence time is 20～100min, and reaction temperature is 5 DEG C～30 DEG C；Described trim,ethylchlorosilane is 1:10～50 with the mass ratio of methyl hydrogen dichlorosilane, and described trim,ethylchlorosilane and the chlorosilane mixture of methyl hydrogen dichlorosilane composition are 1:20～100 with the mass ratio of dilute hydrochloric acid；
Step 2: separating in the oleic acid mixture entrance oleic acid piece-rate system that hydrolysis obtains, after separation, upper strata obtains hydrolysate, and lower floor obtains diluted acid；The described upper strata hydrolysate time of staying in oleic acid piece-rate system is 50～150min；The hydrolysising reacting system that described lower floor diluted acid enters in described step 1 recycles further；Described upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system, enters in dewatering system and carry out processed after the deacidification of described hydrolysate；
Step 3: carrying out containing hydrogen silicone oil telomerisation in the hydrolysate of processed enters equipped with the fixed bed reaction system of catalyst, the temperature of described telomerisation controls at 20～60 DEG C, and the time of telomerizing controls 2～6h；The containing hydrogen silicone oil obtained through telomerisation enters removing impurity in filtration system, enters de-low molecule device from filter containing hydrogen silicone oil out and deviates from low molecule；The hydrolysis circulating reaction system of the low molecule described step 1 of entrance of described abjection recycles further；The described de-low time is 5min～60min, and temperature controls at 100 DEG C～120 DEG C；De-low after containing hydrogen silicone oil enter in containing hydrogen silicone oil refining system and refine, high hydrogeneous containing hydrogen silicone oil can be obtained；The hydrogen content of the described containing hydrogen silicone oil obtained is 1.56～1.60wt%.
Hydrolysis circulating reaction system in described step 1 is made up of venturi mixer, static mixer, heat exchanger, hydrolysis circulating pump.
The dilute hydrochloric acid concentration that in described step 1, hydrolysis uses is 1～5wt%.
In described step 2, water wash system is made up of coalescer and oil-water decanter.
Catalyst in described step 3 is one or both the mixture in Emathlite, strong-acid ion exchange resin.
De-low molecule device in described step 3 is any one of rotating scraper evaporator, falling film evaporator, decompression stirred tank, vaporizer or the combination of two kinds.
Subtractive process in described step 3 includes using activated carbon adsorption and filter to filter.
Further, the one during the material of described coalescer filter element is glass fibre, polyester fiber, metallic fiber, sintering felt, polypropylene fiber, polyster fibre.
Further, the material of described filter element includes polyurethane and polyester fiber.
The beneficial effect comprise that: the raw material hydrolysis that the present invention uses hydrolysis blood circulation to make to produce high containing hydrogen silicone oil can be carried out in low quality concentration hydrochloric acid solution；Use static mixer, these static equipments of venturi-type eductors that the energy consumption of hydrolytic process is substantially reduced, using addition coalescer in water wash system to carry out oil-water separation makes the number of times of washing reduce, the efficiency of washing is greatly improved, avoid the emulsion in water-washing process, improve the yield of high containing hydrogen silicone oil, so that high containing hydrogen silicone oil production cost prepared by this technique is substantially reduced；Meanwhile, hydrolysis blood circulation shortens the high containing hydrogen silicone oil time of staying in concentrated acid so that the hydrogen content of containing hydrogen silicone oil prepared by this technique is maintained between 1.56～1.60wt%.
Accompanying drawing explanation
Fig. 1 is the production technological process of the present invention.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 1wt% is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 20min, temperature is 8 DEG C；Described trim,ethylchlorosilane is 1:10 with the mass ratio of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:30 with the mass ratio of the dilute hydrochloric acid that concentration is 1wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata is hydrolysate, and lower floor is the dilute hydrochloric acid of 16wt%；Described lower floor diluted acid enters hydrolysising reacting system and is circulated utilization；The described upper strata hydrolysate time of staying in oleic acid piece-rate system is 50min；Described upper strata hydrolysate enters water wash system and washes, and removes the acid in hydrolysate；Upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters and carries out containing hydrogen silicone oil telomerisation equipped with in the fixed bed reaction system that catalyst is Emathlite, telomerizes temperature and controls at 50 DEG C, and the time of telomerizing controls at 4h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule, the low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, the de-low time is 20min, temperature controls at 120 DEG C, de-low after containing hydrogen silicone oil enter in containing hydrogen silicone oil refining system and refine, high hydrogeneous containing hydrogen silicone oil can be obtained.The viscosity of the containing hydrogen silicone oil product of preparation is 18(25 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.59wt%.
Embodiment 2
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 3wt% is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 40min, temperature is 12 DEG C；Described trim,ethylchlorosilane is 1:20 with the mass ratio of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:40 with the mass ratio of the dilute hydrochloric acid that concentration is 3wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 20wt%；Lower floor's diluted acid enters hydrolysising reacting system and recycles；The upper strata hydrolysate time of staying in oleic acid piece-rate system is 80min, and upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system, is dehydrated subsequently in dewatering system；
3) hydrolysate through dehydration enters and carries out containing hydrogen silicone oil telomerisation equipped with in the fixed bed reaction system that catalyst is Emathlite, telomerizes temperature and controls at 60 DEG C, and the time of telomerizing controls at 3h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule, the low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 50min, temperature controls at 100 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.58 wt %.
Embodiment 3
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 5wt% is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 30min, temperature is 20 DEG C；Described trim,ethylchlorosilane is 1:30 with the mass ratio of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:80 with the mass ratio of the dilute hydrochloric acid that concentration is 5wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 22wt%, and wherein the hydrolysate time of staying in oleic acid piece-rate system is 100min；Upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system；Lower floor's diluted acid enters hydrolysising reacting system and recycles, and upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters and carries out containing hydrogen silicone oil telomerisation equipped with in the fixed bed reaction system that catalyst is Emathlite, telomerizes temperature and controls at 30 DEG C, and the time of telomerizing controls at 6h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule；The low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 30min, and temperature controls at 120 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.59wt%.
Embodiment 4
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 5wt % is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 90min, temperature is 10 DEG C；Described trim,ethylchlorosilane is 1:45 with the mass ratio of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:90 with the mass ratio of the dilute hydrochloric acid that concentration is 5wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 21wt%, and wherein the hydrolysate time of staying in oleic acid piece-rate system is 120min；Upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system；Lower floor's diluted acid enters hydrolysising reacting system and recycles, and upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters and carries out containing hydrogen silicone oil telomerisation equipped with in the fixed bed reaction system that catalyst is strong-acid ion exchange resin, telomerizes temperature and controls at 60 DEG C, and the time of telomerizing controls at 3h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule；The low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 60min, and temperature controls at 100 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.57 wt %.
Embodiment 5
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 4wt % is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 90min, temperature is 10 DEG C；Described trim,ethylchlorosilane is 1:50 with the mass ratio of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:60 with the mass ratio of the dilute hydrochloric acid that concentration is 4wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 25wt%, and wherein the hydrolysate time of staying in oleic acid piece-rate system is 100min；Upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system；Lower floor's diluted acid enters hydrolysising reacting system and recycles, and upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters and carries out containing hydrogen silicone oil telomerisation equipped with in the fixed bed reaction system that catalyst is strong-acid ion exchange resin, telomerizes temperature and controls at 30 DEG C, and the time of telomerizing controls at 6h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule；The low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 60min, and temperature controls at 105 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.59wt%.
Embodiment 6
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 3wt % is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 90min, temperature is 6 DEG C；Described trim,ethylchlorosilane is 1:40 with the quality of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:75 with the mass ratio of the dilute hydrochloric acid that concentration is 3wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 20wt%, and wherein the hydrolysate time of staying in oleic acid piece-rate system is 120min；Upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system；Lower floor's diluted acid enters hydrolysising reacting system and recycles, and upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters and carries out containing hydrogen silicone oil telomerisation equipped with in the fixed bed reaction system that catalyst is strong-acid ion exchange resin, telomerizes temperature and controls at 40 DEG C, and the time of telomerizing controls at 5h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule；The low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 60min, and temperature controls at 110 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.60 wt %.
Embodiment 7
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 3wt % is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 90min, temperature is 15 DEG C；Described trim,ethylchlorosilane is 1:40 with the quality of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:70 with the mass ratio of the dilute hydrochloric acid that concentration is 3wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 20wt%, and wherein the hydrolysate time of staying in oleic acid piece-rate system is 125min；Upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system；Lower floor's diluted acid enters hydrolysising reacting system and recycles, and upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters equipped with carrying out containing hydrogen silicone oil telomerisation in the fixed bed reaction system of Emathlite and strong-acid ion exchange resin mixed catalyst, telomerizes temperature and controls at 40 DEG C, and the time of telomerizing controls at 6h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule；The low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 50min, and temperature controls at 110 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.60 wt %.
Embodiment 8
The production technology of a kind of continuous prodution height containing hydrogen silicone oil comprises the following steps:
1) low molecule the dilute hydrochloric acid that trim,ethylchlorosilane, methyl hydrogen dichlorosilane, concentration are 3wt % is that raw material is proportionally added into hydrolyzing in circulating reaction system, and mean residence time 100min, temperature is 12 DEG C；Described trim,ethylchlorosilane is 1:45 with the quality of methyl hydrogen dichlorosilane, and the chlorosilane mixture of trim,ethylchlorosilane and methyl hydrogen dichlorosilane composition is 1:80 with the mass ratio of the dilute hydrochloric acid that concentration is 3wt%；
2) oleic acid mixture obtained through hydrolysis separates in oleic acid piece-rate system, and upper strata obtains hydrolysate, and lower floor obtains the dilute hydrochloric acid of 20wt%, and wherein the hydrolysate time of staying in oleic acid piece-rate system is 120min；Upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system；Lower floor's diluted acid enters hydrolysising reacting system and recycles, and upper strata hydrolysate enters in dewatering system and is dehydrated；
3) hydrolysate through dehydration enters equipped with carrying out containing hydrogen silicone oil telomerisation in the fixed bed reaction system of Emathlite and strong-acid ion exchange resin mixed catalyst, telomerizes temperature and controls at 35 DEG C, and the time of telomerizing controls at 6h；Containing hydrogen silicone oil through telomerisation enters and removes impurity in filtration system；Enter de-low molecule device from filter containing hydrogen silicone oil out and deviate from low molecule；The low molecule of described abjection enters in hydrolysis circulating reaction system and recycles further, de-low time 60min, and temperature controls at 120 DEG C, de-low after containing hydrogen silicone oil enter and refined 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 DEG C, mm2/ s), pH value is 7.0, and hydrogen content is 1.60 wt %.
Claims (6)
1. the production technology of a continuous prodution height containing hydrogen silicone oil, it is characterised in that described production technology comprises the following steps:
Step 1: be that raw material joins in hydrolysis circulating reaction system by a certain percentage by trim,ethylchlorosilane, methyl hydrogen dichlorosilane, the low molecule of dilute hydrochloric acid, mean residence time is 20～100min, and reaction temperature is 5 DEG C～30 DEG C；Described trim,ethylchlorosilane is 1:10～50 with the mass ratio of methyl hydrogen dichlorosilane, and described trim,ethylchlorosilane and the chlorosilane mixture of methyl hydrogen dichlorosilane composition are 1:20～100 with the mass ratio of dilute hydrochloric acid；
Step 2: separating in the oleic acid mixture entrance oleic acid piece-rate system that hydrolysis obtains, after separation, upper strata obtains hydrolysate, and lower floor obtains diluted acid；The described upper strata hydrolysate time of staying in oleic acid piece-rate system is 50～150min；The hydrolysising reacting system that described lower floor diluted acid enters in described step 1 recycles further；Described upper strata hydrolysate enters and removes the acid in hydrolysate in water wash system, enters in dewatering system and carry out processed after the deacidification of described hydrolysate；
Step 3: carrying out containing hydrogen silicone oil telomerisation in the hydrolysate of processed enters equipped with the fixed bed reaction system of catalyst, the temperature of described telomerisation controls at 20～60 DEG C, and the time of telomerizing controls 2～6h；The containing hydrogen silicone oil obtained through telomerisation enters removing impurity in filtration system, enters de-low molecule device from filter containing hydrogen silicone oil out and deviates from low molecule；The hydrolysis circulating reaction system of the low molecule described step 1 of entrance of described abjection recycles further；The described de-low time is 5min～60min, and temperature controls at 100 DEG C～120 DEG C；De-low after containing hydrogen silicone oil enter in containing hydrogen silicone oil refining system and refine, high hydrogeneous containing hydrogen silicone oil can be obtained；The hydrogen content of the described containing hydrogen silicone oil obtained is 1.56～1.60wt%；
Hydrolysis circulating reaction system in described step 1 is made up of venturi mixer, static mixer, heat exchanger, hydrolysis circulating pump；
The dilute hydrochloric acid concentration that in described step 1, hydrolysis uses is 1～5wt%；
In described step 2, water wash system is made up of coalescer and oil-water decanter.
The production technology of a kind of continuous prodution height containing hydrogen silicone oil the most according to claim 1, it is characterised in that the catalyst in described step 3 is one or both the mixture in Emathlite, strong-acid ion exchange resin.
The production technology of a kind of continuous prodution height containing hydrogen silicone oil the most according to claim 1, it is characterised in that the de-low molecule device in described step 3 is any one of rotating scraper evaporator, falling film evaporator, decompression stirred tank, vaporizer or the combination of two kinds.
The production technology of a kind of continuous prodution height containing hydrogen silicone oil the most according to claim 1, it is characterised in that the subtractive process in described step 3 includes using activated carbon adsorption and filter to filter.
The production technology of a kind of continuous prodution height containing hydrogen silicone oil the most according to claim 1, it is characterised in that the material of described coalescer filter element is the one in glass fibre, polyester fiber, metallic fiber, sintering felt, polypropylene fiber, polyster fibre.
The production technology of a kind of continuous prodution height containing hydrogen silicone oil the most according to claim 4, it is characterised in that the material of described filter element includes polyurethane and polyester fiber.
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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 |
| 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 |
| CN107417920B (en) * | 2017-09-01 | 2020-08-28 | 合盛硅业股份有限公司 | System and method for producing high-hydrogen-content 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 |
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