CN109970610A - A kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent - Google Patents
A kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent Download PDFInfo
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- CN109970610A CN109970610A CN201910209401.0A CN201910209401A CN109970610A CN 109970610 A CN109970610 A CN 109970610A CN 201910209401 A CN201910209401 A CN 201910209401A CN 109970610 A CN109970610 A CN 109970610A
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- CN
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- preparation
- coupling agent
- production method
- sodium
- thiocarboxylate silane
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- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 title claims abstract description 29
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 25
- 239000007822 coupling agent Substances 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 14
- -1 sulfonyl sodium salt Chemical class 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 11
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000003444 phase transfer catalyst Substances 0.000 claims abstract description 8
- 238000010521 absorption reaction Methods 0.000 claims abstract description 7
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000009471 action Effects 0.000 claims abstract description 3
- 150000001263 acyl chlorides Chemical class 0.000 claims abstract description 3
- 229920000570 polyether Polymers 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 3
- 125000003545 alkoxy group Chemical group 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 3
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims description 2
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 claims description 2
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 6
- 238000004821 distillation Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 150000003376 silicon Chemical class 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical class [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- REEZZSHJLXOIHL-UHFFFAOYSA-N octanoyl chloride Chemical compound CCCCCCCC(Cl)=O REEZZSHJLXOIHL-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940075933 dithionate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C327/00—Thiocarboxylic acids
- C07C327/02—Monothiocarboxylic acids
- C07C327/04—Monothiocarboxylic acids having carbon atoms of thiocarboxyl groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C327/06—Monothiocarboxylic acids having carbon atoms of thiocarboxyl groups bound to hydrogen atoms or to acyclic carbon atoms to hydrogen atoms or to carbon atoms of an acyclic saturated carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a kind of production methods of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, method includes the following steps: 1) NaHS and acyl chlorides react generation sulfonyl sodium salt under the action of phase transfer catalyst, 2) the sulfonyl sodium that step 1) obtains reacts under phase transfer catalyst with halopropyl triethoxysilane, obtains thiocarboxylate silane；Defoaming agent and defoaming class solvent is added in step 1), and reaction kettle is discharged in time by hydrogen sulfide gas is generated using vacuum pump, is then absorbed by the three-level hydrogen sulfide gas absorption plant equipped with saturation sodium hydroxide solution；The volume of reaction kettle can more fully be utilized, increase inventory, reaction time is shortened simultaneously, the yield for greatly promoting product, obtains that color is good, high income and the good product of quality, pollution of the removal of hydrogen sulfide gas to air, the NaHS that absorption kettle generates can be utilized simultaneously, take full advantage of resource, be conducive to industrialized production.
Description
Technical field:
The present invention relates to a kind of production methods of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent.
Background technique:
Silane coupler containing sulfur is the common processing aid of rubber industry, and thiocarboxylate silane's coupling agent of new generation is existing
There is the regeneration product of coupling agent, for compound viscosity can be reduced in the tread rubber of filling white carbon black, reduces and be kneaded number of segment, improve
Sizing material processing performance promotes reinforcing agent dispersion, improves the dynamic mechanical of sizing material.In addition, this coupling agent improves hard charcoal
The ageing-resistant performance of black tread rubber extends sizing material storage time, while also reducing containing for volatile organic matter in finished tire
Amount.The method for synthesizing carbothioic acid ester is more, and wherein NaHS Aqueous phase yield is higher, while because not using solvent, cost
It is lower.Such as 104829645 B of CN discloses the method for preparation thiocarboxylate silane's coupling agent.
Summary of the invention:
Present invention discover that 104829645 B dithionate synthetic reaction process of prior art CN is easy so that raw material overflows
Out, while also reaction time is extended, product quality is affected, causes environmental pollution, its industrialized production is limited, provides
A kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, solves existing technical problem.
The present invention is achieved by the following technical programs:
A kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, this method include following two step
Rapid: 1) NaHS and acyl chlorides react under the action of phase transfer catalyst generates sulfonyl sodium salt, and 2) the obtained sulfonyl of step 1)
Sodium reacts under phase transfer catalyst with halopropyl triethoxysilane, obtains thiocarboxylate silane；Equation is as follows:
Wherein: Y is halogen atom (being selected from F, Cl, Br or I), R1Alkyl, aryl or aralkyl selected from linear chain or branched chain etc.,
R2For hydrogen, alkyl or aralkyl, alkoxy；
It is characterized in that, defoaming agent and defoaming class solvent is added in step 1), and stink damp will be generated using vacuum pump
Reaction kettle is discharged in body in time, is then absorbed by the three-level hydrogen sulfide gas absorption plant equipped with saturation sodium hydroxide solution；Institute
The defoaming agent stated is selected from one or more of polyethers, silicon class, polyether-modified silicon, and the defoaming class solvent is alkane, preferably
Hexamethylene, normal heptane etc..
The polyethers should have excellent water solubility, it is not easy to it is brought into product, such as isomerous tridecanol ether TO-5,
TO-7 etc..
The silicon class should can remove under simple distillation condition, it is not easy to bring into product, such as hexamethyl two
Siloxanes, trimethyl silanol etc..
The polyether modified silicane has good water solubility, while hydrolysis can generate hydroxyl, such as methoxy silane
The polyethers of sealing end, the polyethers etc. of ethyoxyl sealing end.
The defoaming agent addition or defoaming agent and carboxylic acid halides before carboxylic acid halides is added are added simultaneously, preferably the latter, are added simultaneously
The bubble of generation can more fully be eliminated.
The additional amount of defoaming agent is the 5-10wt% of reaction mass.
The small size vacuum water pump, vacuum degree should be advisable with reacting not blistering, and vacuum degree should not be too large, and control as 10-
50 millimetress of mercury.
Particularly, NaHS or vulcanized sodium solid the recycling circulation being precipitated in three-level hydrogen sulfide gas absorption plant are used
It is used as raw material in step 1), avoids environmental pollution, while also having reached recycling for resource, perfectly solves its industry
The problem of metaplasia produces.
Beneficial effects of the present invention are as follows:
1) defoaming agent is added, eliminates or inhibits the generation of bubble in reaction process, prevent the generation of material spray event, simultaneously
It can inhibit the hydrolysis of raw material or product, improve yield.
2) defoaming class solvent is added, such as alkane eliminates the bubble generated in time, while being conducive to water-oil separating, reduces moisture content
And impurity, product loss are smaller.
In short, defoaming agent of the present invention and defoaming class solvent alkane synergistic effect, can more fully utilize reaction kettle
Volume increases inventory, while the preparation duration for shortening sulfonyl sodium greatly promotes product so as to shorten reaction time
Yield, obtain that color is good, high income and the good product of quality, and pollution of the removal of hydrogen sulfide gas to air, while energy
The NaHS that absorption kettle generates is utilized, resource is taken full advantage of, is conducive to industrialized production, solve the prior art
Reaction process raw material is easy to overflow, while also extending reaction time, affects product quality, causes environmental pollution, limits
The problem of its industrialized production.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment 1:
A kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, this method include following two step
It is rapid: 1) pure water to be added in a kettle, turn on agitator puts into NaHS while stirring, stirs ten minutes, complete to solid
Defoaming solution hexamethylene is added after portion's dissolution, reaction solution is down to 10 DEG C hereinafter, opening device for absorbing tail gas with low-temperature circulating pump
And vacuum pump, caprylyl chloride is squeezed into from the first fluid reservoir, opens metering valve, coutroi velocity makes reaction temperature lower than 40 DEG C.
Polyethers defoaming agent TO-5 (5-10wt% that additional amount is reaction mass) is squeezed into from the second fluid reservoir simultaneously, eliminates gas in time
Bubble.The H generated in reaction process2Reaction kettle is discharged in S waste gas utilization vacuum pump in time, then by equipped with saturation sodium hydroxide
The three-level device for absorbing tail gas of solution absorbs, and the NaHS or vulcanized sodium solid being precipitated after saturation can be used as reaction raw materials
It is recycled.After the reaction was completed, liquid reaction obtained imports sedimentation kettle by pipeline, by water phase by lower layer separation row
Fall, calcium chloride water removal is added.It is filtered after stirring one hour and imports distillation still distillation, evaporated before being received by receiving tank 1, receiving tank 2
Collect product.2) the sulfonyl sodium that step 1) obtains reacts under phase transfer catalyst with halopropyl triethoxysilane, obtains
Thiocarboxylate silane, equation are as follows:
Wherein: Y Cl, R1Selected from octyl, R2For hydrogen, alkyl or aralkyl, alkoxy.
Embodiment 2:
A kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, this method include following two step
It is rapid: pure water to be added in a kettle, turn on agitator puts into NaHS while stirring, stirs ten minutes, to solid whole
After dissolution be added defoaming solution normal heptane, with low-temperature circulating pump by reaction solution be down to 10 DEG C hereinafter, open device for absorbing tail gas and
Vacuum pump squeezes into caprylyl chloride from the first fluid reservoir, opens metering valve, and coutroi velocity makes reaction temperature lower than 40 DEG C.Together
When by organic silicon defoaming agent hexamethyldisiloxane (MM) 5-10wt% of reaction mass (additional amount be) from the second fluid reservoir
It squeezes into, eliminates bubble in time.The H generated in reaction process2Reaction kettle is discharged in S waste gas utilization vacuum pump in time, then passes through
Three-level device for absorbing tail gas equipped with saturation sodium hydroxide solution absorbs, the NaHS or vulcanized sodium solid being precipitated after saturation
It can be used as reaction raw materials recycling.After the reaction was completed, liquid reaction obtained imports sedimentation kettle by pipeline, by water phase
It is exhausted by lower layer's separation, calcium chloride water removal is added.It is filtered after stirring one hour and imports distillation still distillation, connect by receiving tank 1
It is evaporated before receipts, receiving tank 2 collects product.2) the sulfonyl sodium that step 1) obtains under phase transfer catalyst with halopropyl triethoxy
Silane reaction obtains thiocarboxylate silane.
Comparative example 1: reference implementation example 1, the difference is that defoaming agent is not added.
Comparative example 2: reference implementation example 1, the difference is that defoaming agent and defoaming class solvent is not added.
Comparative example 3: reference implementation example 1, the difference is that defoaming class solvent is not added.
1 reaction process items correlation data of table
As it can be seen from table 1 the use of defoaming agent and defoaming solution shortens the preparation duration of sulfonyl sodium, the two is common
It is best using defoaming effect.The yield of product also has promotion by a relatively large margin after addition defoaming agent and defoaming solution, this be because
It can inhibit the hydrolysis of product to a certain extent for the defoaming agent of selection, while be conducive to water-oil separating, product loss is smaller.Choosing
The contact between reactant can be increased with defoaming solution, keep reaction more abundant.In short, the collaboration of defoaming agent and defoaming solution
It uses, overall reaction duration can be shortened, obtain that color is good, high income and the good product of quality.
Claims (9)
1. a kind of production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, this method include following two step
Rapid: 1) NaHS and acyl chlorides react under the action of phase transfer catalyst generates sulfonyl sodium salt, and 2) the obtained sulfonyl of step 1)
Sodium reacts under phase transfer catalyst with halopropyl triethoxysilane, obtains thiocarboxylate silane；Equation is as follows:
Wherein: Y is halogen atom, R1Alkyl, aryl or aralkyl selected from linear chain or branched chain, R2For hydrogen, alkyl or aralkyl,
Alkoxy；It is characterized in that, defoaming agent and defoaming class solvent is added in step 1), and hydrogen sulfide gas will be generated using vacuum pump
Then discharge reaction kettle in time is absorbed by the three-level hydrogen sulfide gas absorption plant equipped with saturation sodium hydroxide solution；It is described
Defoaming agent be selected from one or more of polyethers, silicon class, polyether-modified silicon, the defoaming class solvent be alkane.
2. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent, feature exist according to claim 1
In the additional amount of defoaming agent is the 5-10wt% of reaction mass.
3. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, the polyethers are selected from isomerous tridecanol ether TO-5, any one of TO-7.
4. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, the silicon class is selected from hexamethyldisiloxane, trimethyl silanol.
5. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, the polyether-modified silicon is selected from the polyethers of methoxy silane sealing end or the polyethers of ethyoxyl sealing end.
6. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, the defoaming class solvent is hexamethylene or normal heptane.
7. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, NaHS or vulcanized sodium solid the recycling circulation being precipitated in three-level hydrogen sulfide gas absorption plant are made for step 1)
For raw material.
8. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, the defoaming agent and carboxylic acid halides instill simultaneously from different feed inlets.
9. the production method of sodium hydrosulfide preparation thiocarboxylate silane's coupling agent according to claim 1 or claim 2, feature
It is, the small size vacuum pump vacuum degree control is 10-50 millimetres of mercury.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114570186A (en) * | 2022-03-18 | 2022-06-03 | 南京曙光精细化工有限公司 | Environment-friendly treatment method for tail gas generated in production of sulfur-containing silane coupling agent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829645A (en) * | 2015-02-04 | 2015-08-12 | 景德镇宏柏化学科技有限公司 | Method for preparing thiocarboxylate silane coupling agent |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829645A (en) * | 2015-02-04 | 2015-08-12 | 景德镇宏柏化学科技有限公司 | Method for preparing thiocarboxylate silane coupling agent |
Non-Patent Citations (2)
| Title |
|---|
| 吴树森: "《应用物理化学-界面化学与胶体化学》", 31 August 1993, 高等教育出版社 * |
| 工业毒理学编写组: "《工业毒理学》", 31 March 1978, 上海人民出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114570186A (en) * | 2022-03-18 | 2022-06-03 | 南京曙光精细化工有限公司 | Environment-friendly treatment method for tail gas generated in production of sulfur-containing silane coupling agent |
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