CN113637169B - High-quality organic silicon high-boiling hydrolysis oil and preparation method thereof - Google Patents
High-quality organic silicon high-boiling hydrolysis oil and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention relates to the technical field of organic silicon high-boiling hydrolysis oil, in particular to high-quality organic silicon high-boiling hydrolysis oil and a preparation method thereof, wherein the raw materials of the high-boiling hydrolysis oil comprise organic chlorosilane high-boiling residues and trimethylchlorosilane and are obtained according to the following method: the raw materials are mixed and sequentially hydrolyzed, subjected to acid removal, alkali removal and low-boiling-point substance removal to obtain hydrolyzed oil, and then subjected to membrane separation and activated carbon adsorption to obtain the high-quality organic silicon high-boiling hydrolyzed oil. The method utilizes a mode of combining a membrane separation technology and activated carbon adsorption, can better remove gel substances formed by crosslinking in the hydrolyzed oil, reduce the acid value in the hydrolyzed oil, and improve the light transmittance of the product organosilicon high boiling hydrolyzed oil, and has the characteristics of small viscosity, high light transmittance and low acid value.
Description
Technical Field
The invention relates to the technical field of organic silicon high-boiling hydrolysis oil, in particular to high-quality organic silicon high-boiling hydrolysis oil and a preparation method thereof.
Background
The organic silicon material has excellent high and low temperature resistance and electric insulation performance, and is widely applied to the fields of agriculture, industry, military and the like. The GE company in America invented the technology for synthesizing methyl chlorosilane by a direct method in 1941, and realized industrial production in 1947, the direct method is an important mode for producing methyl chlorosilane by monomer enterprises at home and abroad at present, but a series of side reactions also occur along with the progress of main reaction, and byproducts such as monomethyl trichlorosilane, monomethyl hydrogen-containing chlorosilane, trimethyl chlorosilane, high-boiling residues and the like are generated. With the rapid development of the organosilicon industry, the environmental protection pressure is increased along with the increase of byproducts. The effective utilization of the by-products can not only reduce the production cost of enterprises, but also avoid the environmental pollution.
The organochlorosilane high-boiling residues account for about 4 to 10 percent of the total mass of the product, and have low utilization value and complex composition. The boiling point of each component in the high-boiling-point substance is higher than 80 ℃, the high-boiling-point substance has strong irritation, certain safety risks exist in storage and transportation, and the treatment method is complex, high in cost and high in difficulty. The high-boiling-point substance mainly comprises disilane mixtures with structures of Si-Si, si-O-Si, si-C-Si and the like, wherein the total content of trimethyl trichlorosilane and dimethyl tetrachlorodisilane can reach about 30 to 40 percent, and meanwhile, the high-boiling-point substance also contains a small amount of solid impurity particles such as Cu, al, zn, silicon powder and the like.
The organic chlorosilane high-boiling residue can be prepared into a silicone oil product through hydrolysis or alcoholysis reaction. The Chinese patent application No. CN201611079781.3 has a patent name of high-quality organosilicon high boiling hydrolysis oil and a preparation method thereof, wherein organochlorosilane high boiling residues and trimethylchlorosilane are used as raw materials for hydrolysis, the Chinese patent application No. 201110091851.8 and the patent name of a method for preparing neutral ethoxy high boiling silicon oil by using organosilicon high boiling residues are used as raw materials, and alcoholysis, cracking rearrangement, neutralization and other methods are adopted to obtain the organosilicon high boiling hydrolysis oil, however, the organosilicon high boiling hydrolysis oil prepared by alcoholysis of the organochlorosilane high boiling residues contains a hydroxyl end-capping or alkoxy end-capping structure, is easy to crosslink and structurize under an acid-base condition, and seriously affects the product quality.
The organochlorosilane high-boiling-point substance contains a large amount of high-boiling-point substances with disilane structures such as trichloro, tetrachloro and the like, and crosslinking can be generated in the hydrolysis process to generate gel substances, so that the produced high-boiling hydrolysis oil has the problems of high viscosity, turbidity, high acid value and the like.
Disclosure of Invention
The invention provides high-quality organic silicon high-boiling hydrolysis oil and a preparation method thereof, overcomes the defects of the prior art, and can effectively solve the problems of high viscosity, turbidity and high acid value of the existing high-boiling hydrolysis oil.
One of the technical schemes of the invention is realized by the following measures: the high-quality organic silicon high-boiling pyrolysis oil is prepared from 200 parts by weight of organochlorosilane high-boiling residues and 10-20 parts by weight of trimethylchlorosilane by the following method: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, and slowly dropwise adding 100-120 parts of water into the mixed solution for hydrolysis to obtain hydrolysate; secondly, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 150-170 parts of alkali solution for neutralization, standing and layering, removing the alkali solution on the lower layer to obtain hydrolyzed oil, and heating and vacuumizing the hydrolyzed oil to obtain the hydrolyzed oil without low-boiling-point substances; and thirdly, cooling and membrane separation are carried out on the hydrolyzed oil from which the low-boiling-point substances are removed in sequence, and then activated carbon adsorption is carried out on the hydrolyzed oil permeating the membrane to obtain the high-quality organic silicon high-boiling hydrolyzed oil.
The following is a further optimization or/and improvement of one of the above-mentioned technical solutions of the invention:
the alkali solution is more than one of sodium carbonate, sodium bicarbonate, potassium hydroxide and sodium hydroxide solution.
The membrane is an oleophilic hydrophobic membrane.
In the first step, the dropping speed of water is 50g/h to 200g/h, the hydrolysis temperature is 0 ℃ to 60 ℃ during hydrolysis, and the hydrolysis time is 1h to 3h after the water dropping is finished.
In the second step, the mass concentration of the added alkali solution is 5 to 10 percent, and the neutralization time is 1 to 3 hours.
In the second step, the heating temperature is 100 ℃ to 120 ℃, and the vacuumizing pressure is-0.08 MPa to-0.09 MPa.
The second technical scheme of the invention is realized by the following measures: a preparation method of high-quality organic silicon high-boiling pyrolysis oil comprises the following raw materials of 200 parts of organochlorosilane high-boiling residues and 10-20 parts of trimethylchlorosilane in parts by weight: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, and slowly dropwise adding 100-120 parts of water into the mixed solution for hydrolysis to obtain hydrolysate; secondly, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 150-170 parts of alkali solution for neutralization, standing and layering, removing the alkali solution on the lower layer to obtain hydrolyzed oil, and heating and vacuumizing the hydrolyzed oil to obtain the hydrolyzed oil without low-boiling-point substances; and thirdly, cooling and membrane separation are carried out on the hydrolyzed oil from which the low-boiling-point substances are removed in sequence, and then activated carbon adsorption is carried out on the hydrolyzed oil permeating the membrane to obtain the high-quality organic silicon high-boiling hydrolyzed oil.
The following is further optimization or/and improvement of the second technical scheme of the invention:
the alkali solution is more than one of sodium carbonate, sodium bicarbonate, potassium hydroxide and sodium hydroxide solution.
The membrane is an oleophilic hydrophobic membrane.
In the first step, the dropping speed of water is 50g/h to 200g/h, the hydrolysis temperature is 0 ℃ to 60 ℃ during hydrolysis, and the hydrolysis time is 1h to 3h after the water dropping is finished.
In the second step, the mass concentration of the added alkali solution is 5 to 10 percent, and the neutralization time is 1 to 3 hours.
In the second step, the heating temperature is 100 ℃ to 120 ℃, and the vacuumizing pressure is-0.08 MPa to-0.09 MPa.
According to the invention, the organochlorosilane high-boiling residue and the trimethylchlorosilane which are byproducts in the synthesis of the methylchlorosilane are effectively utilized, and the organochlorosilane high-boiling residue and the trimethylchlorosilane are subjected to hydrolysis reaction to prepare the silicone oil product, so that the production cost of enterprises can be reduced, and the environmental pollution can be avoided; the method comprises the steps of sequentially hydrolyzing organic chlorosilane high-boiling-point substances and trimethylchlorosilane, removing acid, alkali and low-boiling-point substances to obtain hydrolyzed oil, selectively permeating silicon oil with a chain-type structure through a lipophilic hydrophobic membrane by adopting a membrane separation technology, effectively separating gel formed by crosslinking, and finally adsorbing the hydrolyzed oil permeating the membrane by activated carbon to obtain the high-quality organic silicon high-boiling-point hydrolyzed oil.
The method utilizes a mode of combining a membrane separation technology and activated carbon adsorption, can better remove gel substances formed by crosslinking in the hydrolyzed oil, reduce the acid value in the hydrolyzed oil, and improve the light transmittance of the product organosilicon high boiling hydrolyzed oil, and has the characteristics of small viscosity, high light transmittance and low acid value.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The various chemical reagents and chemical articles mentioned in the invention are all the chemical reagents and chemical articles which are well known and commonly used in the prior art, unless otherwise specified; the percentages in the invention are mass percentages unless otherwise specified; the solution in the present invention is an aqueous solution of water as a solvent unless otherwise specified, for example, a hydrochloric acid solution is an aqueous hydrochloric acid solution.
The invention is further described below with reference to the following examples:
example 1: the high-quality organic silicon high-boiling hydrolysis oil comprises the following raw materials, by weight, 200 parts of organochlorosilane high-boiling residues and 10-20 parts of trimethylchlorosilane, and is obtained by the following method: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, and slowly dropwise adding 100-120 parts of water into the mixed solution for hydrolysis to obtain hydrolysate; step two, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 150 to 170 parts of alkali solution for neutralization, standing and layering, removing the alkali solution on the lower layer to obtain hydrolyzed oil, and heating and vacuumizing the hydrolyzed oil to obtain the hydrolyzed oil without low-boiling-point substances; and thirdly, cooling and membrane separation are carried out on the hydrolyzed oil from which the low-boiling-point substances are removed in sequence, and then activated carbon adsorption is carried out on the hydrolyzed oil permeating the membrane to obtain the high-quality organic silicon high-boiling hydrolyzed oil.
In the invention, the raw materials of organochlorosilane high-boiling residue and trimethylchlorosilane are byproducts for synthesizing methylchlorosilane; the type of the membrane is oleophylic and hydrophobic membrane, and the material of the membrane can be inorganic membrane, organic membrane or organic-inorganic composite membrane.
Example 2: in the optimization of the above embodiment, the alkaline solution is one or more of sodium carbonate, sodium bicarbonate, potassium hydroxide and sodium hydroxide solution.
Example 3: as an optimization of the above embodiment, the membrane is an oleophilic hydrophobic membrane.
Example 4: as the optimization of the embodiment, in the first step, the dropping speed of water is 50g/h to 200g/h, the hydrolysis temperature is 0 ℃ to 60 ℃ during hydrolysis, and the hydrolysis time is 1h to 3h after the water drop is completely added.
Example 5: as optimization of the above embodiment, in the second step, the mass concentration of the added alkali solution is 5% to 10%, and the neutralization time is 1h to 3h.
Example 6: as an optimization of the above embodiment, in the second step, the heating temperature is 100 ℃ to 120 ℃, and the vacuum pressure is-0.08 MPa to-0.09 MPa.
Example 7: the high-quality organic silicon high-boiling hydrolysis oil is prepared from 200g of organochlorosilane high-boiling residues and 10g of trimethylchlorosilane by the following method: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, slowly dropwise adding 100g of water into the mixed solution by using a separating funnel for hydrolysis to obtain hydrolysate, wherein the dropwise adding speed of the water is 50g/h, the hydrolysis temperature is 0 ℃ during hydrolysis, and the hydrolysis time is after water drops are completely added, and then continuously carrying out equilibrium reaction for 1h; secondly, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 150g of sodium carbonate solution for neutralization, standing and layering, removing the sodium carbonate solution on the lower layer to obtain hydrolyzed oil, and heating and vacuumizing the hydrolyzed oil to obtain the hydrolyzed oil without low-boiling-point substances, wherein the mass concentration of the added sodium carbonate solution is 5%, the neutralization time is 1h, the heating temperature is 100 ℃, and the vacuumizing pressure is-0.08 MPa; and thirdly, cooling and membrane separating the hydrolyzed oil from which the low-boiling-point substances are removed in sequence, and then carrying out activated carbon adsorption on the hydrolyzed oil penetrating through the membrane to obtain the high-quality organic silicon high-boiling hydrolyzed oil, wherein the membrane is an oleophylic hydrophobic membrane.
Example 8: the high-quality organic silicon high-boiling pyrolysis oil is prepared from 200g of organochlorosilane high-boiling residues and 15g of trimethylchlorosilane by the following steps: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, slowly dropwise adding 120g of water into the mixed solution by using a separating funnel for hydrolysis to obtain hydrolysate, wherein the dropwise adding speed of the water is 200g/h, the hydrolysis temperature is 60 ℃ during hydrolysis, and the hydrolysis time is that after water drops are completely added, continuously carrying out equilibrium reaction for 3h; step two, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 170g of sodium bicarbonate solution for neutralization, standing and layering, removing the sodium bicarbonate solution on the lower layer to obtain hydrolyzed oil, and heating and vacuumizing the hydrolyzed oil to obtain the hydrolyzed oil without low-boiling-point substances, wherein the mass concentration of the added sodium bicarbonate solution is 10%, the neutralization time is 3h, the heating temperature is 120 ℃, and the vacuumizing pressure is-0.09 MPa; and thirdly, cooling and membrane separating the hydrolyzed oil from which the low-boiling-point substances are removed in sequence, and then carrying out activated carbon adsorption on the hydrolyzed oil penetrating through the membrane to obtain the high-quality organic silicon high-boiling hydrolyzed oil, wherein the membrane is an oleophylic hydrophobic membrane.
Example 9: the high-quality organic silicon high-boiling pyrolysis oil is prepared from 200g of organochlorosilane high-boiling residues and 20g of trimethylchlorosilane by the following steps: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, slowly dropwise adding 110g of water into the mixed solution by using a separating funnel for hydrolysis to obtain hydrolysate, wherein the dropwise adding speed of the water is 100g/h, the hydrolysis temperature is 30 ℃ during hydrolysis, and the hydrolysis time is after water drops are completely added, and then continuously carrying out equilibrium reaction for 2h; step two, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 160g of potassium hydroxide solution for neutralization, standing and layering, removing the potassium hydroxide solution on the lower layer to obtain hydrolyzed oil, and heating and vacuumizing the hydrolyzed oil to obtain the hydrolyzed oil without low-boiling-point substances, wherein the mass concentration of the added potassium hydroxide solution is 8%, the neutralization time is 2 hours, the heating temperature is 110 ℃, and the vacuumizing pressure is-0.09 MPa; and thirdly, cooling and membrane separating the hydrolyzed oil from which the low-boiling-point substances are removed in sequence, and then carrying out activated carbon adsorption on the hydrolyzed oil penetrating through the membrane to obtain the high-quality organic silicon high-boiling hydrolyzed oil, wherein the membrane is an oleophylic hydrophobic membrane.
Comparative example 1: the procedure was the same as in example 9 except that activated carbon adsorption was not used in the procedure.
Comparative example 2: the procedure was the same as in example 9 except that no membrane separation was used in the procedure.
The high-quality organic silicon high-boiling boiled oil prepared in the embodiments 7 to 9 of the invention has the characteristics of small viscosity, high light transmittance and low acid value, and the following physical and chemical indexes are considered in the embodiments 7 to 9, the comparative examples 1 and the comparative examples 2, and the physical and chemical indexes comprise: the turbidity degree, viscosity, light transmittance, volatile components and acid value and the turbidity degree are observed by naked eyes, and the rest is detected by referring to a method specified in DB13T2142-2014 organosilicon high boiling hydrolysis oil. The detection results are shown in table 1, and it can be seen from table 1 that the light transmittance of the organosilicon high boiling water hydrolysis oil treated by both the membrane separation and the activated carbon adsorption techniques is higher than that of the organosilicon high boiling water hydrolysis oil treated by only the membrane separation and the activated carbon adsorption techniques, and although the light transmittance of the organosilicon high boiling water hydrolysis oil treated by only the membrane separation and the activated carbon adsorption techniques can be improved, the invention has certain limitations.
In conclusion, the method utilizes a mode of combining a membrane separation technology and activated carbon adsorption, can better remove gel substances formed by crosslinking in the hydrolyzed oil, reduce the acid value in the hydrolyzed oil, and improve the light transmittance of the product organosilicon high-boiling hydrolyzed oil, and has the characteristics of small viscosity, high light transmittance and low acid value.
The technical characteristics form the embodiment of the invention, the embodiment has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual requirements to meet the requirements of different situations.
Claims (1)
1. A preparation method of high-quality organic silicon high-boiling pyrolysis oil is characterized in that the raw materials comprise 200 parts of organochlorosilane high-boiling residues and 10-20 parts of trimethylchlorosilane by weight, and the preparation method comprises the following steps: firstly, uniformly stirring and mixing organochlorosilane high-boiling residues and trimethylchlorosilane in required amount to obtain mixed solution, slowly dropwise adding 100-120 parts of water into the mixed solution for hydrolysis to obtain hydrolysate, wherein the dropwise adding speed of the water is 50-200 g/h, the hydrolysis temperature is 0-60 ℃ during hydrolysis, and the hydrolysis time is that after water drops are completely added, the equilibrium reaction is continuously carried out for 1-3 h; secondly, standing and layering the hydrolysate, removing hydrochloric acid on the lower layer, adding 150 to 170 parts of alkali solution for neutralization, wherein the mass concentration of the added alkali solution is 5 to 10 percent, the alkali solution is more than one of sodium carbonate, sodium bicarbonate, potassium hydroxide and sodium hydroxide solution, the neutralization time is 1 to 3 hours, then standing and layering, removing the alkali solution on the lower layer to obtain hydrolyzed oil, heating the hydrolyzed oil at 100 to 120 ℃, vacuumizing to obtain the hydrolyzed oil with low-boiling-point substances removed, and vacuumizing the pressure to be-0.08 to-0.09 MPa; and thirdly, cooling the hydrolyzed oil without the low-boiling-point substances, separating by using an oleophylic hydrophobic membrane, and adsorbing the hydrolyzed oil penetrating through the membrane by using activated carbon to obtain the high-quality organic silicon high-boiling hydrolyzed oil.
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