CN104231271A - Liquid silicon resin and preparation method and application thereof - Google Patents
Liquid silicon resin and preparation method and application thereof Download PDFInfo
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- CN104231271A CN104231271A CN201410543098.5A CN201410543098A CN104231271A CN 104231271 A CN104231271 A CN 104231271A CN 201410543098 A CN201410543098 A CN 201410543098A CN 104231271 A CN104231271 A CN 104231271A
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Abstract
The invention belongs to the field of synthesis of organosilicone, and specifically relates to liquid silicon resin and a preparation method and application thereof. The liquid silicon resin is particularly applied to the preparation of silicone sealant as a plasticizer replacing simethicone. The preparation method of the liquid silicon resin is prepared through a reaction kettle which is equipped with an agitating device and a condensing reflowing device. The preparation method comprises the following steps: a, preparing raw materials, namely, mixing methyl trichlorosilane and dimethyldichlorosilance, and controlling the temperature of the reaction kettle to be below 5 DEG C; b, dropwise adding and reacting, namely, dropwise adding concentrated hydrochloric acid to the reaction kettle, controlling the temperature of a reaction system to be -10 to 5 DEG C, reacting until no bubble is produced after dropwise adding concentrated hydrochloric acid, and separating oil and water of the reaction system; c, neutralizing oil layer, namely, adding a solid alkaline substance to the oil layer obtained by separating in step b while agitating in order to neutralize the oil layer to reach the neutrality; d, filtering the oil layer, namely, filtering the neutral oil layer obtained in step c, wherein the filtrate is the primary liquid silicon resin; finally refining at low temperature to obtain the refined liquid silicon resin.
Description
Technical field
The invention belongs to organosilicon synthesis field, be specifically related to a kind of liquid silicone resin and its preparation method and application, this liquid silicone resin is particularly useful for preparing silicone sealant.
Background technology
The primary product of direct synthesis organosilane monomer is dimethyldichlorosilane(DMCS), can produce a large amount of by products simultaneously, and wherein dimethyldichlorosilane(DMCS) and METHYL TRICHLORO SILANE are topmost two compositions, account for 85% ~ 88% and 10% ~ 15% respectively.
Dimethyldichlorosilane(DMCS) and METHYL TRICHLORO SILANE all have boiling point lower, easy volatilization and transport difficult, again because himself molecular weight greatly and easily forms vapor slugs, meeting naked light can burn or explode, meet water and then produce the defects such as larger hydrogen chloride gas, danger is very large.Current dimethyldichlorosilane(DMCS) can as the raw material of DMC, and for the synthesis of the derived product such as silicon rubber or silicone oil, METHYL TRICHLORO SILANE is then mainly used for various silane coupling agent, silicone resin, water-proof material use.
Current silicone sealant all will use dimethyl silicone oil to be used as softening agent in preparation process, to add more reinforced filling, increase the intensity of silicone rubber products, but because the chemically reactive of dimethyl silicone oil is low, reaction is not participated in system, cause to use in silicone rubber products process in the later stage and there will be slow oil impregnate situation, have extreme influence to the intensity of product and looking products.Therefore, the present inventor replaces dimethyl silicone oil as softening agent for providing the activated liquid silicone of a kind of tool.
Summary of the invention
Technical problem solved by the invention is to provide a kind of liquid silicone replacing dimethyl silicone oil to use as softening agent and preparation method thereof.
The preparation method of liquid silicone of the present invention, carries out, comprises the steps: in the reactor with whipping appts and condensation reflux unit
A, preparation of raw material: mixed methyl trichlorosilane and dimethyldichlorosilane(DMCS), control the temperature of reactor lower than 5 DEG C;
B, dropwise reaction: in reactor, drip concentrated hydrochloric acid, the temperature controlling reaction system is-10 ~ 5 DEG C; Concentrated hydrochloric acid dropwises rear reaction and produces to bubble-free, and reaction system is carried out oily water separation;
C, oil reservoir neutralize: in the separating obtained oil reservoir of step b, add solid-state alkaline matter while stirring and are neutralized to oil reservoir for neutral;
D, filtration oil reservoir: filtration step c obtains neutral oil reservoir, and gained filtrate is primary liquid silicone resin.
Further, refining liquid silicone resin is refined and obtained to primary liquid silicone resin through de-low.
Wherein, de-low refining is: primary liquid silicone resin steps d obtained carries out de-low refining, de-low temperature is 120 ~ 160 DEG C (preferably 140 DEG C), pressure is-0.06 ~-0.09MPa (preferably-0.085MPa), and the de-low time is 2 ~ 4 hours (preferably 4 hours); Namely discharging obtains refining liquid silicone resin.
In order to efficent use of resources, the tail gas reacting generation can also be passed into monomer absorption device, hydrogenchloride retrieving arrangement successively, obtain comparatively pure hydrogen chloride gas in step b.Wherein, monomer absorption device utilizes concentrated hydrochloric acid to absorb the tail gas of escaping out.
In technique scheme, in step a, the mass ratio of dimethyldichlorosilane(DMCS) and METHYL TRICHLORO SILANE is 63 ︰ 7 ~ 27.
In technique scheme, in step b, concentrated hydrochloric acid addition by weight, dimethyldichlorosilane(DMCS) weight is 1.5-2 times (preferably 1.8 times) of concentrated hydrochloric acid consumption, and METHYL TRICHLORO SILANE weight is 2-3 times (preferably 2.5 times) of concentrated hydrochloric acid consumption.That is, the mixture of METHYL TRICHLORO SILANE and dimethyldichlorosilane(DMCS) and the weight ratio of concentrated hydrochloric acid are 1.8-2.3 (preferably 2 times).
In technique scheme, the speed dripping concentrated hydrochloric acid in step b is 0.8 ~ 1.5kg/h; Preferred 1.1kg/h.Controlling rate of addition is adopt constant pressure dropping funnel, controls at the uniform velocity to drip.Dripping too fast meeting causes reaction uneven, and the by product of generation is many, drips and wastage of material productive rate can be caused slowly not high, and the molecular weight product of generation is comparatively large, is unfavorable for later-stage utilization.
In technique scheme, the reaction end of step b produces with bubble-free to be as the criterion, and the usual reaction times is at 0.5-1 hour.
In technique scheme, the concentration of concentrated hydrochloric acid described in step b is 33 ~ 37%.
In technique scheme, condensation reflux unit is the prolong of jacketed, when dripping concentrated hydrochloric acid, passing into refrigerant and carrying out heat exchange cooling in chuck.Wherein, the preferred ethylene glycol of described refrigerant.Concrete operations are passed in chuck by freezing ethylene glycol to cool.
In technique scheme, in step b, the temperature controlling reaction system utilizes the condensing temperature controlling condensate recycling device to control lower than-10 DEG C.
In technique scheme, in step c, alkaline matter is one or more in sodium carbonate, sodium hydroxide, sodium bicarbonate.
The present invention refines liquid silicone resin, can replace dimethyl silicone oil as softening agent for Formula type silicone rubber products such as silicone sealants, have economic worth widely.Because primary liquid silicone resin contains more lower-molecular substance or dimethyl polysiloxane mixed methylcyclosiloxane, therefore directly should not be used as softening agent.In addition, in preparation process, adopt concentrated hydrochloric acid to be added drop-wise in chlorosilane mixed system the reaction that is hydrolyzed, farthest can reduce the generation of the rear spent acid of reaction.Preparation method of the present invention can also obtain comparatively pure hydrogen chloride gas, can use as the raw material of other chemical process.
The invention has the beneficial effects as follows: the mode of being reacted by dropping concentrated hydrochloric acid and mix monomer, filtered by standing separation, neutralization, the measure such as de-low refining and tail gas recycle, primary liquid silicone resin, refining liquid silicone resin and concentrated hydrochloric acid three kinds of products can be obtained.Elementary and refining liquid silicone resin tool has been widely used and higher marketable value, and gained concentration of hydrochloric acid is greater than 33%, can return use.Gained refines the problem that liquid silicone resin can also solve dimethyl silicone oil in silicone sealant preparation process, substitutes dimethyl silicone oil and uses as softening agent.
Accompanying drawing explanation
Fig. 1 is present invention process schema
Embodiment
Illustrate below by way of specific description of embodiments of the present invention but do not limit the present invention.
As shown in Figure 1, the preparation method of liquid silicone resin of the present invention, the reactor of employing, with stirring and condensation reflux unit, comprises the steps:
A, preparation of raw material: METHYL TRICHLORO SILANE and dimethyl dichloro silicon in mass ratio 63 ︰ 7 ~ 27 are mixed to get mix monomer.And the temperature of reactor is reduced to less than 5 DEG C.Cooling can adopt cold cycle groove to carry out cooling process to raw material.
B, dropwise reaction: in reactor, drip concentrated hydrochloric acid, the temperature controlling reaction system can not exceed-10 ~ 5 DEG C.Concentrated hydrochloric acid dropwises rear reaction and produces to bubble-free, and reaction system is carried out oily water separation.
The concentration of concentrated hydrochloric acid is preferably 33 ~ 37%.The speed that concentrated hydrochloric acid drips can suitably adjust according to the velocity of discharge of tail gas, and the time preferably dripping concentrated hydrochloric acid is 2 ~ 3 hours.Pass into freezing ethylene glycol carry out heat exchange to changing in condensing works during preferred dropping hydrochloric acid, control the condensing temperature of condensate recycling device simultaneously below-10 DEG C.Along with the carrying out of reaction, the volatilization of a large amount of hydrogenchloride can make temperature of reaction system reduce, and takes part chlorosilane monomer out of, and condensing works can make the chlorosilane monomer of taking out of be condensed to get back in reactor until react completely.To feed in raw material rear continuation reaction 0.5 ~ 1 hour.Utilize liquid distributing device to be separated profit after leaving standstill, get oil reservoir.The reaction mainly carried out in this step is:
C, oil reservoir neutralize: in the separating obtained oil reservoir of step b, add solid-state alkaline matter while stirring and are neutralized to oil reservoir for neutral;
The liquid be obtained by reacting in step b has very strong acidity, is a kind of very unstable product.If not in time except disacidify can be cross-linked very soon.The alkaline matter that deacidification adopts is one or more in sodium carbonate, sodium hydroxide, sodium bicarbonate, should open large stirring as far as possible in N-process, with in accelerating and speed.
D, filtration oil reservoir: filtered by the neutral oil reservoir obtained in step c, gained filtrate is primary liquid silicone resin.
The oil reservoir obtained in step c is mixed with a large amount of salinity, the oily mater that outward appearance is creamy white, and just can obtain product after needing salinity to filter.Filtration can take natural filtration, also can adopt press filtration or suction filtration.The filtrate obtained is oily liquids, is primary liquid silicone resin.
De-low refining: the primary liquid silicone resin in steps d to be carried out de-low refining.Concrete, Rotary Evaporators can be adopted to process, de-low temperature 120 ~ 160 DEG C, pressure is-0.06 ~-0.09MPa; Namely discharging obtains product.
Containing a lot of lower-molecular substances in the primary liquid silicone resin obtained in steps d, these materials will reduce the intensity of silicone rubber products in later-stage utilization, take off low so need to carry out high temperature.De-low can select autoclave take off low, rotate de-low, film and take off the modes such as low.What contriver adopted according to existence conditions is rotate de-low, and de-low condition is de-low temperature 120 ~ 160 DEG C, and pressure is-0.06 ~-0.09MPa, 2 ~ 4 hours time.Preferred de-low condition is de-low temperature 140 DEG C, and pressure is-0.085MPa, 4 hours time.
Tail gas recycle: the tail gas reacting generation in step b is passed into monomer absorption device, hydrogenchloride retrieving arrangement successively.
React expellant gas in step b and be mainly dimethyldichlorosilane(DMCS), METHYL TRICHLORO SILANE, hydrogenchloride.During concrete enforcement, device for absorbing tail gas, containing two covering devices, is respectively: a set of monomer absorption device and a set of hydrogenchloride retrieving arrangement.Wherein monomer absorption device is used for absorbing hydrogen chloride gas entrainment monomer out.
Below by embodiment, the specific embodiment of the present invention is described further, but not therefore by protection scope of the present invention restriction in one embodiment.
Embodiment one
The mass ratio of dimethyldichlorosilane(DMCS) and METHYL TRICHLORO SILANE is 9 ︰ 1; Hydrolysis temperature 0 DEG C; Adopt sodium carbonate neutralization, de-low temperature 140 DEG C, pressure-0.06MPa.
Add the mix monomer raw material of 500 volumes in a kettle., be cooled to 0 DEG C, drip the concentrated hydrochloric acid of 200 volumes while stirring.Dropwise after 2 hours, leave standstill bubble-free after 0.5 hour and produce, layering, release the hydrochloric acid bottom reactor, the concentration of hydrochloric acid separated is 35%.In oil reservoir, add sodium carbonate solid be neutralized to neutrality, cross leaching filtrate and carry out rotary distillation 3 hours, the de-low temperature 140 DEG C of control, pressure-0.06MPa obtain product.Viscosity is 86mm
2/ s, refractive index 1.39, at 150 DEG C, 3 hours fugitive constituents are 1.3%.
Be used for silicone sealant experiment by through de-low product, the product tensile strength obtained arrives 1.4MPa, and elongation at break reaches 650%.
Embodiment two
The mass ratio of dimethyldichlorosilane(DMCS) and METHYL TRICHLORO SILANE is 4 ︰ 1; Hydrolysis temperature-5 DEG C; Adopt sodium bicarbonate neutralization, de-low temperature 130 DEG C, pressure-0.09MPa.
Add the mix monomer raw material of 500 volumes in a kettle., be cooled to-5 DEG C, while stirring from the concentrated hydrochloric acid of dropping 200 volume.Dropwise after 2 hours, leave standstill bubble-free after 0.5 hour and produce, layering, release the hydrochloric acid bottom reactor, the concentration of hydrochloric acid separated is 33%.In oil reservoir, add sodium bicarbonate solid be neutralized to neutrality, cross leaching filtrate and carry out rotary distillation 3 hours, the de-low temperature 130 DEG C of control, pressure-0.09MPa obtain product.Viscosity is 115mm
2/ s, refractive index 1.41, at 150 DEG C, 3 hours fugitive constituents are 1.9%.
Be used for silicone sealant experiment by through de-low product, the product tensile strength obtained arrives 1.6MPa, and elongation at break reaches 620%.
Claims (10)
1. the preparation method of liquid silicone resin, carries out in the reactor with whipping appts and condensation reflux unit, it is characterized in that comprising the steps:
A, preparation of raw material: mixed methyl trichlorosilane and dimethyldichlorosilane(DMCS), control the temperature of reactor lower than 5 DEG C;
B, dropwise reaction: in reactor, drip concentrated hydrochloric acid, the temperature controlling reaction system is-10 ~ 5 DEG C; Concentrated hydrochloric acid dropwises rear reaction and produces to bubble-free, and reaction system is carried out oily water separation;
C, oil reservoir neutralize: in the separating obtained oil reservoir of step b, add solid-state alkaline matter while stirring and are neutralized to oil reservoir for neutral;
D, filtration oil reservoir: filtration step c obtains neutral oil reservoir, and gained filtrate is primary liquid silicone resin.
2. the preparation method of liquid silicone resin according to claim 1, is characterized in that: refining liquid silicone resin is refined and obtained to steps d gained primary liquid silicone resin through de-low;
Preferably, the described de-low primary liquid silicone resin refined as steps d being obtained carries out de-low refining, and de-low temperature is 120 ~ 160 DEG C, and pressure is-0.06 ~-0.09MPa, and the de-low time is 2 ~ 4 hours, and namely discharging obtains refining liquid silicone resin.
3. the preparation method of the liquid silicone resin according to any one of claim 1 or 2, is characterized in that: in step a, the mass ratio of dimethyldichlorosilane(DMCS) and METHYL TRICHLORO SILANE is 63 ︰ 7 ~ 27.
4. the preparation method of the liquid silicone resin according to any one of claim 1 or 2, it is characterized in that: in step b, concentrated hydrochloric acid addition by weight, dimethyldichlorosilane(DMCS) weight is 1.5-2 times of concentrated hydrochloric acid consumption, and METHYL TRICHLORO SILANE weight is 2-3 times of concentrated hydrochloric acid consumption;
Preferably, dimethyldichlorosilane(DMCS) weight is 1.8 times of concentrated hydrochloric acid consumption;
Preferably, METHYL TRICHLORO SILANE weight is 2.5 times of concentrated hydrochloric acid consumption;
Preferably, the mixture of METHYL TRICHLORO SILANE and dimethyldichlorosilane(DMCS) and the weight ratio of concentrated hydrochloric acid are 1.8-2.3;
Preferably, the mixture of METHYL TRICHLORO SILANE and dimethyldichlorosilane(DMCS) and the weight ratio of concentrated hydrochloric acid are 2.
5. the preparation method of the liquid silicone resin according to any one of claim 1 or 2, is characterized in that: the speed dripping concentrated hydrochloric acid in step b is 0.8 ~ 1.5kg/h; Preferred 1.1kg/h.
6. the preparation method of the liquid silicone resin according to any one of claim 1 or 2, is characterized in that: pass into refrigerant carry out heat exchange to changing in condensing works when dripping concentrated hydrochloric acid in step b; The preferred ethylene glycol of described refrigerant.
7. the preparation method of the liquid silicone resin according to any one of claim 1 or 2, is characterized in that: the temperature controlling reaction system described in step b utilizes the condensing temperature controlling condensate recycling device to control lower than-10 DEG C.
8. the preparation method of the liquid silicone resin according to any one of claim 1 or 2, is characterized in that: alkaline matter described in step c is one or more in sodium carbonate, sodium hydroxide, sodium bicarbonate.
9. the preparation method described in any one of claim 1-8 prepares gained liquid silicone resin.
10. liquid silicone resin described in claim 9 is as the application of softening agent;
Preferably, liquid silicone resin is as the application of softening agent preparing silicone sealant.
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Cited By (3)
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| CN106629604A (en) * | 2016-11-28 | 2017-05-10 | 昆明理工大学 | Method for preparing gas-phase hydrogen chloride by utilizing chlorosilane residue |
| CN111801369A (en) * | 2018-12-28 | 2020-10-20 | 浙江三时纪新材科技有限公司 | Polysiloxane powder without pungent smell during heating and preparation method thereof |
| US10815339B2 (en) | 2016-04-26 | 2020-10-27 | Guangdong Biomax Si&F New Material Co., Ltd. | Method for preparing organopolysiloxane resins |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10815339B2 (en) | 2016-04-26 | 2020-10-27 | Guangdong Biomax Si&F New Material Co., Ltd. | Method for preparing organopolysiloxane resins |
| CN106629604A (en) * | 2016-11-28 | 2017-05-10 | 昆明理工大学 | Method for preparing gas-phase hydrogen chloride by utilizing chlorosilane residue |
| CN106629604B (en) * | 2016-11-28 | 2019-07-16 | 昆明理工大学 | A method of gas phase chlorination hydrogen is produced using chlorosilane raffinate |
| CN111801369A (en) * | 2018-12-28 | 2020-10-20 | 浙江三时纪新材科技有限公司 | Polysiloxane powder without pungent smell during heating and preparation method thereof |
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