CN106117049A - A kind of method of the residual comprehensive utilization of dichlorohydrin still - Google Patents
A kind of method of the residual comprehensive utilization of dichlorohydrin still Download PDFInfo
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- CN106117049A CN106117049A CN201610467244.XA CN201610467244A CN106117049A CN 106117049 A CN106117049 A CN 106117049A CN 201610467244 A CN201610467244 A CN 201610467244A CN 106117049 A CN106117049 A CN 106117049A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/02—Preparation of carboxylic acid esters by interreacting ester groups, i.e. transesterification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
- C07C29/1285—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis of esters of organic acids
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The invention belongs to the Waste Disposal Technology field produced in chemical process, a kind of method being specifically related to residual comprehensive utilization of dichlorohydrin still.The method technological operation is simple, makes full use of dangerous solid waste and produces value-added product, makes dangerous solid waste obtain Appropriate application, adds the economic benefit of enterprise, both economically and environmentally beneficial.
Description
Technical field
The invention belongs to the Waste Disposal Technology field produced in chemical process, be specifically related to a kind of dichlorohydrin
The method of the residual comprehensive utilization of still.
Background technology
Dichlorohydrin is important industrial chemicals and intermediate, for the synthesis of antiviral agents ganciclovir, as acetic acid
Fiber, the solvent of ethyl cellulose, be also used for manufacturing epoxy resin, ion exchange resin etc..
This enterprise uses the method for crude glycerine chlorination to prepare dichlorohydrin, and the crude product obtained is through rectification isolated dichloro third
Alcohol product.It is raw material owing to using crude glycerine, the most about contains 0.9% glyceryl monostearate, 0.8% pair of glycerol stearate
Ester, 1.3% glyceryl stearate mixture and 2% sodium chloride, in chlorination process, tristerin is not involved in reaction, single hard
Glycerol, glycerol distearate generate dichloro tristerin, a chlorine tristerin respectively.Dichlorohydrin is thick
Still that product rectification obtains is residual middle about contains 15% 1 chlorine tristerin, 13% dichloro tristerin, 22% stearic acid
Glyceride, 3%3-chloro-1,2-propylene glycol, 35% sodium chloride and 12% tar.This enterprise produces dichlorohydrin about 80,000 tons per year, every year
Produce residual about 4000 tons of dichlorohydrin still.At present, dichlorohydrin still is residual is that the producer delivering to qualification as dangerous solid waste is carried out
High temperature continuous pyrolysis burning disposal, still per ton residual burning disposal expense is up to 7000-8000 unit, not only increases the negative of enterprise
Load, environment is also caused secondary pollution by burning disposal simultaneously, is unfavorable for environmental conservation.
Summary of the invention
It is an object of the invention to: a kind of method that residual comprehensive utilization of dichlorohydrin still is provided, the method technological operation letter
Single, make full use of dangerous solid waste and produce value-added product, make dangerous solid waste obtain Appropriate application, add the economic effect of enterprise
Benefit, both economically and environmentally beneficial.
The technical solution of the present invention is: is 1. dissolved by residual for dichlorohydrin still organic solvent, is filtrated to get chlorine
Changing sodium solid organic solvent at room temperature to wash, cleaning mixture set, for the residual dissolving of still of lower batch, washs afterchlorinate sodium
Obtaining concentration 20% sodium chloride solution with water dissolution, solution filters removes a small amount of water-insoluble, and filtrate obtains after removing a small amount of solvent
To meeting the concentration about 23% sodium-chloride water solution (TOC≤100ppm) that electrolysis requires, filtrate recycling design set is for lower batch
The residual dissolving of secondary still；Tar therein is carried out adsorbing, filtering by the filtrate that the most Isolating chlorinated sodium obtains with adsorbent, and filter cake is dried
Recycling design set is for the residual dissolving of still of lower batch；3. the filtrate that tar removing obtains adds a certain amount of catalyst, in uniform temperature
Under carry out ester exchange reaction, after the reactant liquor normal pressure that obtains removing excessive solvent, rectification under vacuum obtains 1,3 (2,3)-dichlorohydrins,
More than still, liquid stratification obtains lower floor 3-chloro-1,2-propylene glycol and crude glycerine mixed liquor goes to carry out the synthesis of dichlorohydrin；4.
The upper strata reactant liquor arrived removes catalyst through washing, and after washing, feed liquid l00 DEG C air-distillation goes out the water of remnants, still material warp after dehydration
Rectification under vacuum obtains stearate.
Organic solvent of the present invention is alcohol organic solvent, preferably methanol, ethanol, more preferably methanol；
Organic solvent of the present invention and the residual mass ratio of dichlorohydrin still are 0.5～5:1, preferably 1～3:1, more preferably 1
～2:1；
Organic solvent solution temperature of the present invention is 0～80 DEG C, preferably 30～70 DEG C, more preferably 50～60 DEG C；
Organic solvent dissolution time of the present invention is 1～8 hour, preferably 2～6 hours, more preferably 3～4 hours；
Organic solvent used by washing solid sodium chloride of the present invention is 1～5:1 with the mass ratio of sodium chloride, preferably 1
～2:1；
The present invention uses the purpose that solvent dissolution kettle is residual: after tar and organic component are dissolved by (1), during separation and recovery still is residual
Salt, thus realize the recycling of salt；(2) this solvent also acts as the work of ester exchange agent in follow-up ester exchange reaction
With.Therefore, the present invention uses organic solvent, and adsorbent is the most merely separating tar, also acts as separation, reclaims salt and realization
The effect of Organic substance comprehensive utilization.
Adsorbent of the present invention is activated carbon or kieselguhr, preferably activated carbon；
Tar adsorption adsorbent of the present invention is 0.01～0.1:1 with the mass ratio of filtrate, preferably 0.03～0.08:
1, more preferably 0.05～0.06:1；
Adsorbent tar temperature of the present invention is 0～80 DEG C, preferably 30～70 DEG C, more preferably 50～60 DEG C；
The adsorbent tar time of the present invention is 1～8 hour, preferably 2～6 hours, more preferably 3～4 hours；
Ester exchange catalyst of the present invention is inorganic base or mineral acid, and inorganic base catalyst is Lithium hydrate, hydrogen-oxygen
Changing sodium, potassium hydroxide, inorganic acid catalyst is sulphuric acid, phosphoric acid, preferably potassium hydroxide, sulphuric acid；
Ester exchange catalyst consumption of the present invention is the 0.1～2% of decoking amount of filtrate, preferably 0.5～1.5%, more
Preferably 0.8～1%；
Transesterification reaction temperature of the present invention is 0～70 DEG C, preferably 30～60 DEG C, more preferably 40～50 DEG C；
The ester exchange reaction time of the present invention is 1～6 hour, preferably 2～5 hours, more preferably 3～4 hours；
The ester exchange upper strata of the present invention reactant liquor washing water yield is 0.1～1:1 with the mass ratio of reactant liquor, preferably
0.2～0.5:1.
In the present invention, the purpose of ester exchange is hard to available Organic substance one chlorine tristerin in residual for still, dichloro
Glycerol, tristerin, 3-chlorine-1,2-propylene glycol comprehensively utilize, and reclaim the most merely and obtain 1,3 (2,3)-two
Chloropropyl alcohol product, has also reclaimed raw material 3-chlorine-1,2-propylene glycol and the crude glycerine preparing dichlorohydrin, by-product stearic acid first simultaneously
Ester, ethyl ester.
The invention have the advantage that (1) technological operation is simple, it is achieved that Organic substance separates with inorganic matter and comprehensive utilization,
Exploitativeness is strong；(2) make full use of dangerous solid waste and produce value-added product, bring economic benefit to enterprise, both economically and environmentally beneficial.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these embodiments are intended merely to
Illustrate the present invention, rather than limit the scope of the present invention by any way.
Embodiment 1
By in residual for 1000g dichlorohydrin still input 2000ml four-hole bottle, addition 1000g methanol is warming up to 50 DEG C and is incubated
Dissolving, dissolution time is 4 hours, and the complete mixed liquor of insulation is down to room temperature and is filtered, and obtains faint yellow solid sodium chloride 380g, palm fibre
Color filtrate 1615g.Solid sodium chloride respectively with 400g methanol be stirred at room temperature washing 2 times, obtain cleaning mixture 795g set under
The residual dissolving of still of batch, washing afterchlorinate sodium 378g water dissolution obtains concentration about 20% sodium chloride solution, and solution crosses elimination
Except water-insoluble 3g, it is met, after filtrate normal pressure removing 33g methanol, concentration about 23% sodium-chloride water solution that electrolysis requires
1500g (TOC=85ppm), reclaims the residual dissolving of still for lower batch of the methanol set.
The brown filtrate 1615g obtained by Isolating chlorinated sodium joins in 2000ml four-hole bottle, and adds kieselguhr 80g,
Being warming up to 60 DEG C of insulations and within 4 hours, carry out tar absorption, the complete mixed liquor of insulation is down to room temperature and is filtered, and obtains the diatom containing tar
Soil 280g, dries recovery methanol about 80g and goes the residual dissolving of still, obtain pale yellow filtrate 1405g；
The filtrate 1405g obtained by tar removing puts in 2000ml four-hole bottle, adds potassium hydroxide 10g, is warming up to 50
DEG C insulation reaction carries out ester exchange reaction in 4 hours, obtains the methanol 771g 64 DEG C of abjection excess under reactant liquor normal pressure, obtains
Mixed liquor, in 2mmHg, rectification under the conditions of 90～110 DEG C, obtains 1,3 (2,3)-dichlorohydrin 53g.More than rectifying still, liquid is layered obtains
Removing synthesizing dichloropropanol to lower floor's 3-chlorine-1,2-propylene glycol and crude glycerine mixed liquor 129g, its composition respectively may be about 40% He
60%, obtain upper strata reactant liquor 460g；
Upper strata reactant liquor 460g washs 2 times with 150g water the most respectively, removes a small amount of catalyst, obtains cleaning mixture
305g.After washing, esterifying liquid 455g goes out the water 5g of remnants l00 DEG C of air-distillation, and still clout liquid is at 2mmHg, 170～180 DEG C of bars
Under part, rectification obtains methyl stearate 440g, and content is more than 99%.
Embodiment 2
By in residual for 1000g dichlorohydrin still input 2000ml four-hole bottle, addition 1200g ethanol is warming up to 60 DEG C and is incubated
Dissolving, dissolution time is 3 hours, and the complete mixed liquor of insulation is down to room temperature and is filtered, and obtains faint yellow solid sodium chloride 392g, palm fibre
Color filtrate 1806g.Solid sodium chloride respectively with 500g ethanol be stirred at room temperature washing 2 times, obtain cleaning mixture 996g set under
The residual dissolving of still of batch, washing afterchlorinate sodium 385g water dissolution obtains concentration about 20% sodium chloride solution, and solution crosses elimination
Except water-insoluble 3g, it is met, after filtrate normal pressure removing 38g ethanol, concentration about 23% sodium-chloride water solution that electrolysis requires
1500g (TOC=73ppm), reclaims the residual dissolving of still for lower batch of the ethanol set.
The brown filtrate 1806g obtained by Isolating chlorinated sodium joins in 2000ml four-hole bottle, and adds activated carbon 100g,
Being warming up to 50 DEG C of insulations and within 4 hours, carry out tar absorption, the complete mixed liquor of insulation is down to room temperature and is filtered, and obtains the activity containing tar
Charcoal 320g, dries recovery ethanol about 100g and goes the residual dissolving of still, obtain pale yellow filtrate 1581g；
The filtrate 1581g obtained by tar removing puts in 2000ml four-hole bottle, adds concentrated sulphuric acid 15g, is warming up to 40 DEG C
Insulation reaction carries out ester exchange reaction in 3 hours, obtains the ethanol 923g 78 DEG C of abjection excess under reactant liquor normal pressure, and obtain is mixed
Close liquid in 2mmHg, rectification under the conditions of 90～110 DEG C, obtain 1,3 (2,3)-dichlorohydrin 52.5g.More than rectifying still, liquid is layered obtains
Removing synthesizing dichloropropanol to lower floor's 3-chlorine-1,2-propylene glycol and crude glycerine mixed liquor 128.5g, its composition respectively may be about 41% He
59%, obtain upper strata reactant liquor 487g；
Upper strata reactant liquor 487g washs 2 times with 150g water the most respectively, removes a small amount of catalyst, obtains cleaning mixture
308g.After washing, esterifying liquid 479g goes out the water 6g of remnants l00 DEG C of air-distillation, and still clout liquid is at 2mmHg, 170～180 DEG C of bars
Under part, rectification obtains ethyl stearte 455g, and content is more than 99%.
Embodiment 3
By in residual for 1000g dichlorohydrin still input 5000ml four-hole bottle, addition 1500g methanol is warming up to 60 DEG C and is incubated
Dissolving, dissolution time is 3 hours, and mixed liquor is down to room temperature and is filtered, and obtains faint yellow solid sodium chloride 376g, brown filtrate
2118g.Solid sodium chloride is stirred at room temperature washing 2 times with 750g methanol respectively, obtains cleaning mixture 1490g and overlaps for lower batch
The residual dissolving of still, washing afterchlorinate sodium 371g water dissolution obtains concentration about 20% sodium chloride solution, and solution filters removes water not
Molten thing about 3g, is met, after filtrate normal pressure removing 22g methanol, concentration about the 23% sodium-chloride water solution 1500g that electrolysis requires
(TOC=61ppm) the residual dissolving of still for lower batch of the methanol set, is reclaimed.
The brown filtrate 2118g obtained by Isolating chlorinated sodium joins in 2000ml four-hole bottle, and adds activated carbon 120g,
Being warming up to 50 DEG C of insulations and within 4 hours, carry out tar absorption, the complete mixed liquor of insulation is down to room temperature and is filtered, and obtains the activity containing tar
Charcoal 361g, dries recovery methanol about 120g and goes the residual dissolving of still, obtain pale yellow filtrate 1872g；
The filtrate 1872g obtained by tar removing puts in 2000ml four-hole bottle, adds concentrated sulphuric acid 15g, is warming up to 60 DEG C
Insulation reaction carries out ester exchange reaction in 4 hours, obtains the methanol 1229g 64 DEG C of abjection excess under reactant liquor normal pressure, obtains
Mixed liquor, in 2mmHg, rectification under the conditions of 90～110 DEG C, obtains 1,3 (2,3)-dichlorohydrin 50g.More than rectifying still, liquid is layered obtains
Removing synthesizing dichloropropanol to lower floor's 3-chlorine-1,2-propylene glycol and crude glycerine mixed liquor 129g, its composition respectively may be about 41.5% He
58.5%, obtain upper strata reactant liquor 468g；
Upper strata reactant liquor 468g washs 2 times with 150g water the most respectively, removes a small amount of catalyst, obtains cleaning mixture
310g.After washing, esterifying liquid 458g goes out the water 7g of remnants l00 DEG C of air-distillation, and still clout liquid is at 2mmHg, 170～180 DEG C of bars
Under part, rectification obtains methyl stearate 437g, and content is more than 99%.
Embodiment 4
By in residual for 1000g dichlorohydrin still input 2000ml four-hole bottle, addition 500g methanol is warming up to 60 DEG C and is incubated
Dissolving, dissolution time is 4 hours, and mixed liquor is down to room temperature and is filtered, and obtains brown color solid sodium chloride 410g, brown filtrate
1086g.Solid sodium chloride is stirred at room temperature washing 3 times with 600g methanol respectively, obtains cleaning mixture 1792g and overlaps for lower batch
The residual dissolving of still, washing afterchlorinate sodium 392g water dissolution obtains concentration about 20% sodium chloride solution, and solution filters removes water not
Molten thing about 3g, obtains meeting concentration about 23% sodium-chloride water solution that electrolysis requires after filtrate normal pressure removing 31g methanol
1500g (TOC=330ppm), reclaims the residual dissolving of still for lower batch of the methanol set.
The brown filtrate 1086g obtained by Isolating chlorinated sodium joins in 2000ml four-hole bottle, and adds activated carbon 60g,
Being warming up to 50 DEG C of insulations and within 4 hours, carry out tar absorption, the complete mixed liquor of insulation is down to room temperature and is filtered, and obtains the activity containing tar
Charcoal 250g, dries recovery methanol about 60g and goes the residual dissolving of still, obtain yellow filtrate 890g；
The filtrate 890g obtained by tar removing puts in 2000ml four-hole bottle, adds sodium hydroxide 8g, is warming up to 60 DEG C
Insulation reaction carries out ester exchange reaction in 3 hours, obtains the methanol 262g 64 DEG C of abjection excess under reactant liquor normal pressure.Obtain is mixed
Close liquid in 2mmHg, rectification under the conditions of 90～110 DEG C, obtain 1,3 (2,3)-dichlorohydrin 51.5g.More than rectifying still, liquid is layered obtains
Removing synthesizing dichloropropanol to lower floor's 3-chlorine-1,2-propylene glycol and crude glycerine mixed liquor 126.5g, its composition respectively may be about 42% He
58%, obtain upper strata reactant liquor 458g；
Upper strata reactant liquor 458g washs 2 times with 150g water the most respectively, removes a small amount of catalyst, obtains cleaning mixture
304g.After washing, esterifying liquid 454g goes out the water 5g of remnants l00 DEG C of air-distillation, and still clout liquid is at 2mmHg, 170～180 DEG C of bars
Under part, rectification obtains methyl stearate 421g, and content is more than 99%.
Claims (10)
1. the method for the residual comprehensive utilization of dichlorohydrin still, it is characterised in that 1. residual for dichlorohydrin still organic solvent is entered
Row dissolves, and is filtrated to get solid sodium chloride organic solvent and at room temperature washs, and cleaning mixture set is residual for the still of lower batch
Dissolving, washing afterchlorinate sodium water dissolution obtains concentration 20% sodium chloride solution, and solution filters removes a small amount of water-insoluble, filtrate
Being met the concentration about 23% sodium-chloride water solution (TOC≤100ppm) that electrolysis requires after removing a small amount of solvent, filtrate is returned
Receive the residual dissolving of still for lower batch of the solvent set；Tar therein is inhaled by the filtrate that the most Isolating chlorinated sodium obtains with adsorbent
Attached, filtration, filter cake dries the residual dissolving of still for lower batch of the recycling design set；3. the filtrate that tar removing obtains adds a certain amount of urging
Agent, carries out ester exchange reaction at a certain temperature, and after the reactant liquor normal pressure removing excessive solvent obtained, rectification under vacuum obtains 1,3
(2,3)-dichlorohydrin, liquid stratification obtains lower floor's 3-chlorine-1,2-propylene glycol and crude glycerine mixed liquor goes to carry out dichloro more than still
The synthesis of propanol；4. the upper strata reactant liquor obtained removes catalyst through washing, and after washing, feed liquid l00 DEG C air-distillation goes out remnants'
Water, after dehydration, still material obtains stearate through rectification under vacuum.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described organic solvent
It is alcohol organic solvent, preferably methanol, ethanol.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described organic solvent
Mass ratio residual with dichlorohydrin still is 0.5～5:1, preferably 1～3:1, more preferably 1～2:1.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described organic solvent
Solution temperature is 0～80 DEG C, preferably 30～70 DEG C, more preferably 50～60 DEG C；Described organic solvent dissolution time is 1～8 little
Time, preferably 2～6 hours, more preferably 3～4 hours.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described washing chlorination
Organic solvent used by sodium solid is 1～5:1 with the mass ratio of sodium chloride, preferably 1～2:1.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described adsorbent is
Activated carbon or kieselguhr.Described adsorbent is 0.01～0.1:1 with the mass ratio of filtrate, preferably 0.03～0.08:1, more preferably
0.05～0.06:1.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described adsorbent is inhaled
Attached tar temperature is 0～80 DEG C, preferably 30～70 DEG C, more preferably 50～60 DEG C；The described adsorbent tar time be 1～
8 hours, preferably 2～6 hours, more preferably 3～4 hours.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described ester exchange is urged
Agent is inorganic base or mineral acid, and inorganic base catalyst is Lithium hydrate, sodium hydroxide, potassium hydroxide, and inorganic acid catalyst is
Sulphuric acid, phosphoric acid.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described ester exchange is urged
Agent consumption is the 0.1～2% of decoking amount of filtrate, preferably 0.5～1.5%, more preferably 0.8～1%；Described ester exchange reaction
Temperature is 0～70 DEG C, preferably 30～60 DEG C, more preferably 40～50 DEG C；The described ester exchange reaction time is 1～6 hour, preferably
2～5 hours, more preferably 3～4 hours.
The method of the residual comprehensive utilization of dichlorohydrin still the most according to claim 1, it is characterised in that described ester exchange
The upper strata reactant liquor washing water yield is 0.1～1:1 with the mass ratio of reactant liquor, preferably 0.2～0.5:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156726A (en) * | 2019-06-03 | 2019-08-23 | 江苏扬农化工集团有限公司 | A kind of method of the residual comprehensive utilization of epoxychloropropane rectifying still |
| CN110963509A (en) * | 2019-12-08 | 2020-04-07 | 浙江大洋生物科技集团股份有限公司 | Method for disposing waste residues generated in amprolium hydrochloride condensation procedure |
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| SU1030355A1 (en) * | 1982-04-23 | 1983-07-23 | Предприятие П/Я Р-6751 | Process for recovering and purifying polyglycerins and salt from bottoms of glycerin production |
| CN105237354A (en) * | 2014-10-24 | 2016-01-13 | 连云港环海化工有限公司 | Glycerin chlorination residual liquid recycling method |
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| SU1030355A1 (en) * | 1982-04-23 | 1983-07-23 | Предприятие П/Я Р-6751 | Process for recovering and purifying polyglycerins and salt from bottoms of glycerin production |
| CN105237354A (en) * | 2014-10-24 | 2016-01-13 | 连云港环海化工有限公司 | Glycerin chlorination residual liquid recycling method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156726A (en) * | 2019-06-03 | 2019-08-23 | 江苏扬农化工集团有限公司 | A kind of method of the residual comprehensive utilization of epoxychloropropane rectifying still |
| CN110963509A (en) * | 2019-12-08 | 2020-04-07 | 浙江大洋生物科技集团股份有限公司 | Method for disposing waste residues generated in amprolium hydrochloride condensation procedure |
| CN110963509B (en) * | 2019-12-08 | 2022-08-12 | 浙江大洋生物科技集团股份有限公司 | Method for disposing waste residues generated in amprolium hydrochloride condensation procedure |
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