CN102030905B - Method for preparing solvent-free high hydrogen containing silicone oil - Google Patents
Method for preparing solvent-free high hydrogen containing silicone oil Download PDFInfo
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- CN102030905B CN102030905B CN2010105735699A CN201010573569A CN102030905B CN 102030905 B CN102030905 B CN 102030905B CN 2010105735699 A CN2010105735699 A CN 2010105735699A CN 201010573569 A CN201010573569 A CN 201010573569A CN 102030905 B CN102030905 B CN 102030905B
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- silicone oil
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- containing hydrogen
- hydrogen silicone
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 38
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 38
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 19
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000000292 calcium oxide Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 22
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 9
- 239000012266 salt solution Substances 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 235000012255 calcium oxide Nutrition 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 208000006558 Dental Calculus Diseases 0.000 claims description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000002685 polymerization catalyst Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 7
- 238000002156 mixing Methods 0.000 abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000000178 monomer Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000005046 Chlorosilane Substances 0.000 abstract description 2
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 abstract description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 abstract description 2
- 230000004931 aggregating effect Effects 0.000 abstract 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 150000002431 hydrogen Chemical class 0.000 description 24
- 239000012535 impurity Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000004902 Softening Agent Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920000260 silastic Polymers 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004758 synthetic textile Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention relates to a method for preparing solvent-free high hydrogen containing silicone oil, belonging to the field of chemical engineering and comprising the following steps of: adding methyl dichloresilane and methyl chlorosilane as raw materials in proportion in an agitated reactor, mixing uniformly; on the premise of stirring, adding excessive inorganic salt or hydrochloric acid or a mixed solution of inorganic salt or hydrochloric acid in the agitated reactor at a certain speed, controlling the temperature in the agitated reactor, keeping the temperature to be -5 DEG C-4 DEG C until the reaction is ended, standing and demixing, drying upper components with anhydrous sodium carbonate or sodium bicarbonate or calcium oxide and neutralizing remained acid; and aggregating the dried and neutralized upper components, and removing low-boiling-point substances to obtain the solvent-free high hydrogen containing silicone oil. The invention avoids using the solvent toluene when the high hydrogen containing silicone oil is synthesized by using chlorosilane monomers in the traditional process, saves the energy sources, lowers the pollution to the environment, and can obtain an excellent-quality product with transparent appearance, high hydrogen content and no solvent odor.
Description
Technical field
The present invention relates to a kind of method for preparing solvent-free high containing hydrogen silicone oil, belong to chemical field.
Background technology
High containing hydrogen silicone oil has many particular performances, like fabulous thermostability, chemicalstability, water repellency and reactivity etc.These particular performances make high containing hydrogen silicone oil be used widely in a lot of fields, like antifouling, grease proofing, the waterproof finishing agent as building; The raw material of preparation modified silicon oil is used for natural and synthetic fabrics, silk, the water-resisting agent of leather and the textile auxiliary agent of softening agent; The waterproof of paper, release agent; The waterproof softening agent of spun glass; The linking agent of liquid silastic; Anti-yellow agent of high-temperature mixing glue or the like.
The raw material dimethyl dichlorosilane (DMCS) of high containing hydrogen silicone oil is one of by product of methyl chlorosilane monomer device generation.That the hydrogeneous monomer of dimethyl dichlorosilane (DMCS) has is inflammable and explosive, corrodibility strong, be difficult for the characteristics of preserving, and deals with improperly and very easily causes safety and environmental protection hidden danger.Produce solvent-free high containing hydrogen silicone oil and not only can handle by product, can also create favorable economic benefit, avoid environmental pollution.
Prior art is many with solvent method production, and is residual unavoidably when removing solvent, makes high containing hydrogen silicone oil degradation.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of method for preparing solvent-free high containing hydrogen silicone oil is provided.The present invention has avoided the pollution that solvent toluene brought in the traditional technology, and can obtain the quality products of appearance transparent, high hydrogen content, solvent-free flavor.
In order to achieve the above object, the technical scheme of the present invention's employing is:
A kind of method for preparing solvent-free high containing hydrogen silicone oil may further comprise the steps:
(1) in proportion material dimethyl dichlorosilane (DMCS), trimethylchlorosilane are added reaction kettle, stir;
(2) under the prerequisite that stirs, with excess inorganic salts solution or hydrochloric acid or inorganic salt hydrochloric acid mixed solution adding reaction kettle, the control reactor temperature remains between-5～45 ℃;
(3) stop to reaction, standing demix, with the upper strata component with yellow soda ash or sodium hydrogencarbonate or quicklime is dry and in and acid residues;
(4) the upper strata component that step (3) is obtained removes low-boiling-point substance, promptly gets solvent-free high containing hydrogen silicone oil.
2. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1 is characterized in that, in the step (1), the material ratio is carried out proportioning according to viscosity, the molecular-weight average of required high containing hydrogen silicone oil.
3. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1 is characterized in that, in the step (2), inorganic salt can be yellow soda ash, sodium sulfate, vitriolate of tartar, calcium chloride, sodium-chlor, Repone K; Inorganic salt solution concentration is 5% to saturated; Concentration of hydrochloric acid is 5-37%.
4. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1 is characterized in that, in the step (2), the control method of reactor temperature is: initial reaction stage is thermo-negative reaction to mid-term, need not temperature control; The reaction middle and later periods is thermopositive reaction, cooling maintains the temperature at-5-45 ℃ between.
5. like the method for claim 1 or the solvent-free high containing hydrogen silicone oil of 4 described preparations; It is characterized in that; In the step (2); Reaction just, mid-term can water, inorganic salt solution, hydrochloric acid or its three's arbitrary combination direct reaction, and the reaction later stage is with inorganic salt solution, hydrochloric acid or the two arbitrary combination direct reaction.
6. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1; It is characterized in that, in the step (4), before the upper strata component that step (3) is obtained removes low-boiling-point substance; Can add polymerization catalyst earlier; Polymerizing condition is: under the prerequisite that adds catalyzer and 20-60 ℃ of condition, reacted 2-6 hour, catalyzer is that concentration is sulfuric acid or Zeo-karb or the acidic white earth of 70-98%.
The present invention compared with prior art uses solvent when having avoided with the synthetic high containing hydrogen silicone oil of chlorosilane monomer, and save energy has reduced the pollution to environment, and make that product appearance is good, free from extraneous odour, hydrogen content be high.
Embodiment
Below in conjunction with embodiment the present invention is detailed.
Embodiment 1:
1000kg dimethyl dichlorosilane (DMCS), 15kg trimethylchlorosilane are added reaction kettle, mixing.The flow of control inorganic salt hydrochloric acid soln keeps reactor temperature not surpass 45 ℃, when system no longer includes hydrogen chloride gas and emits, and layering, washing, with dried over anhydrous sodium carbonate, neutralization.Product under 20～60 ℃ of conditions, with strongly acidic cationic exchange resin catalyzed reaction 1～6 hour, after the filtration, is removed low molecule and impurity and gets under negative pressure, high containing hydrogen silicone oil.
Embodiment 2:
500kg dimethyl dichlorosilane (DMCS), 10kg trimethylchlorosilane are added reaction kettle, mixing.Keep reactor temperature-5～45 ℃, dominant discharge adds the soft water of 1/2 metering, adds the inorganic salt hydrochloric acid soln with certain flow then, finishes until reaction.With in the reactants dry and after, under 20～60 ℃ of conditions,, after the filtration, under negative pressure, remove low molecule and impurity with acidic white earth catalyzed reaction 1～6 hour, promptly get high containing hydrogen silicone oil.
Embodiment 3:
500kg dimethyl dichlorosilane (DMCS), 6kg trimethylchlorosilane are added reaction kettle, and control inorganic salt hydrochloric acid soln flow keeps reactor temperature not surpass 45 ℃, when system no longer includes hydrogen chloride gas and emits, and layering, dry with quicklime.Adding concentration and be 70～98% sulfuric acid is catalyzer, and reaction is 6 hours under 20～60 ℃ of conditions, and catalyst neutralisation removes low molecule, impurity, high containing hydrogen silicone oil.
Embodiment 4:
500kg dimethyl dichlorosilane (DMCS), 7.5kg trimethylchlorosilane are added reaction kettle, mixing.Keep reactor temperature-5～45 ℃, add the inorganic salt hydrochloric acid soln, finish until reaction with certain flow.Adding concentration and be 70～90% sulfuric acid is catalyzer, under 20～60 ℃ of conditions, reacts 2～6 hours, and catalyst neutralisation removes low molecule, impurity, high containing hydrogen silicone oil.
Embodiment 5:
500kg dimethyl dichlorosilane (DMCS), 6kg trimethylchlorosilane are added reaction kettle, and control inorganic salt hydrochloric acid soln flow keeps reactor temperature not surpass 45 ℃, when system no longer includes hydrogen chloride gas and emits, and layering, dry with quicklime.Remove low molecule, impurity, get high containing hydrogen silicone oil.
Embodiment 6:
Keep reactor temperature-5～45 ℃, add the inorganic salt hydrochloric acid soln, behind 500kg dimethyl dichlorosilane (DMCS), 7.5kg trimethylchlorosilane mixing, add reaction kettle with certain flow.Finish until reaction, adding concentration and be 70～90% sulfuric acid is catalyzer, under 20～60 ℃ of conditions, reacts 2～6 hours, and catalyst neutralisation removes low molecule, impurity, high containing hydrogen silicone oil.
Embodiment 7:
Keep reactor temperature-5～45 ℃, add the inorganic salt hydrochloric acid soln.Dominant discharge behind 500kg dimethyl dichlorosilane (DMCS), 10kg trimethylchlorosilane mixing, adds reaction kettle with certain speed.With reactant with in the sodium hydrogencarbonate and after, under negative pressure, remove low molecule and impurity, promptly get high containing hydrogen silicone oil.
Claims (2)
1. method for preparing solvent-free high containing hydrogen silicone oil is characterized in that it may further comprise the steps:
(1) in proportion material dimethyl dichlorosilane (DMCS), trimethylchlorosilane are added reaction kettle, stir; The material ratio is carried out proportioning according to viscosity, the molecular-weight average of required high containing hydrogen silicone oil;
(2) under the prerequisite that stirs, with excess inorganic salts solution or hydrochloric acid or inorganic salt hydrochloric acid mixed solution adding reaction kettle, the control reactor temperature remains between-5～45 ℃;
(3) stop to reaction, standing demix, with the upper strata component with yellow soda ash or sodium hydrogencarbonate or quicklime is dry and in and acid residues;
(4) the upper strata component that step (3) is obtained removes low-boiling-point substance, promptly gets solvent-free high containing hydrogen silicone oil.
2. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1 is characterized in that, in the step (2), inorganic salt are yellow soda ash, sodium sulfate, vitriolate of tartar, calcium chloride, sodium-chlor, Repone K; Inorganic salt solution concentration is 5% to saturated; Concentration of hydrochloric acid is 5-37%.
3. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1 is characterized in that, in the step (2), the control method of reactor temperature is: initial reaction stage is thermo-negative reaction to mid-term, need not temperature control; The reaction middle and later periods is thermopositive reaction, cooling maintains the temperature at-5-45 ℃ between.
4. like the method for claim 1 or the solvent-free high containing hydrogen silicone oil of 3 described preparations; It is characterized in that; In the step (2); Reaction just, mid-term water, inorganic salt solution, hydrochloric acid or its three's arbitrary combination direct reaction, the reaction later stage is with inorganic salt solution, hydrochloric acid or the two arbitrary combination direct reaction.
5. the method for the solvent-free high containing hydrogen silicone oil of preparation as claimed in claim 1; It is characterized in that, in the step (4), before the upper strata component that step (3) is obtained removes low-boiling-point substance; Add polymerization catalyst earlier; Polymerizing condition is: under the prerequisite that adds catalyzer and 20-60 ℃ of condition, reacted 2-6 hour, catalyzer is that concentration is sulfuric acid or Zeo-karb or the acidic white earth of 70-98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105735699A CN102030905B (en) | 2010-12-06 | 2010-12-06 | Method for preparing solvent-free high hydrogen containing silicone oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105735699A CN102030905B (en) | 2010-12-06 | 2010-12-06 | Method for preparing solvent-free high hydrogen containing silicone oil |
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| Publication Number | Publication Date |
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| CN102030905A CN102030905A (en) | 2011-04-27 |
| CN102030905B true CN102030905B (en) | 2012-10-31 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516545B (en) * | 2011-11-11 | 2013-08-07 | 江苏创基新材料有限公司 | Method for continuously producing hydrogen-containing silicon oil |
| CN102643428A (en) * | 2012-04-27 | 2012-08-22 | 泸州北方化学工业有限公司 | Method for preparing methyl hydrogen polysiloxane oil |
| CN103131010A (en) * | 2013-04-01 | 2013-06-05 | 唐山三友硅业有限责任公司 | Silicone oil preparation method by means of simultaneous hydrolysis of high-boiling residues and low-boiling residues of organic silicon |
| CN103554502B (en) * | 2013-10-23 | 2016-05-04 | 泸州北方化学工业有限公司 | No-solvent type containing hydrogen silicone oil and preparation method thereof |
| CN103923319B (en) * | 2014-04-08 | 2016-03-30 | 吉林华丰有机硅有限公司 | The method of high containing hydrogen silicone oil is produced in the solvent-free hydrolysis of monomethyl dichlorosilane |
| CN105085921B (en) * | 2015-08-19 | 2018-09-07 | 湖北兴瑞化工有限公司 | A method of preparing Methyl Hydrogen Polysiloxane Fluid using organic silicon byproduct |
| CN106366316A (en) * | 2016-08-30 | 2017-02-01 | 唐山三友硅业有限责任公司 | Method for preparing high-hydrogen-content silicone oil by using methyl dichlorosilane |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101215381B (en) * | 2008-01-14 | 2011-02-16 | 杭州师范大学 | Method for preparing methylphenyl hydrogen-containing silicone oil |
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Address after: 063305 Nanpu Development Zone, Hebei, Tangshan City Patentee after: Tangshan Sanyou Silicon Industry Co.,Ltd. Address before: 063305 Nanpu economic and Technological Development Zone, Hebei, Tangshan City Patentee before: SANYOU SILICON INDUSTRY Co.,Ltd. |