CN114181178A - Method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof - Google Patents
Method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof Download PDFInfo
- Publication number
- CN114181178A CN114181178A CN202111622812.6A CN202111622812A CN114181178A CN 114181178 A CN114181178 A CN 114181178A CN 202111622812 A CN202111622812 A CN 202111622812A CN 114181178 A CN114181178 A CN 114181178A
- Authority
- CN
- China
- Prior art keywords
- alpha
- butyrolactone
- acetyl
- gamma
- chloro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 112
- CYCRRRIREKXQTK-UHFFFAOYSA-N 3-acetyl-3-chlorooxolan-2-one Chemical compound CC(=O)C1(Cl)CCOC1=O CYCRRRIREKXQTK-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000001704 evaporation Methods 0.000 claims abstract description 25
- 238000011084 recovery Methods 0.000 claims abstract description 19
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 11
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 44
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 22
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 22
- OMQHDIHZSDEIFH-UHFFFAOYSA-N 3-Acetyldihydro-2(3H)-furanone Chemical compound CC(=O)C1CCOC1=O OMQHDIHZSDEIFH-UHFFFAOYSA-N 0.000 claims description 16
- 230000008020 evaporation Effects 0.000 claims description 11
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 7
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000005660 chlorination reaction Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 229930003451 Vitamin B1 Natural products 0.000 claims description 4
- 229960003495 thiamine Drugs 0.000 claims description 4
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 claims description 4
- 239000011691 vitamin B1 Substances 0.000 claims description 4
- 235000010374 vitamin B1 Nutrition 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 1
- 238000004821 distillation Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- 238000010612 desalination reaction Methods 0.000 abstract description 5
- 239000011345 viscous material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 25
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 8
- 229910052801 chlorine Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/26—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D307/30—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/32—Oxygen atoms
- C07D307/33—Oxygen atoms in position 2, the oxygen atom being in its keto or unsubstituted enol form
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D415/00—Heterocyclic compounds containing the thiamine skeleton
Abstract
The invention provides a method for recovering alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water and application thereof, relating to the technical field of chemical industry, wherein the recovery method comprises the following steps: neutralizing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone. The invention solves the technical problem that the operation of the environmental protection facility is not smooth due to viscous substances generated when the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water is used as wastewater for distillation desalination treatment, and achieves the technical effects of recovering the alpha-chloro-alpha-acetyl-gamma-butyrolactone from the stratified water, improving the economic benefit and improving the operation efficiency of the environmental protection facility.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for recovering alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water and application thereof.
Background
The existing alpha-chloro-alpha-acetyl-gamma-butyrolactone synthesis process takes alpha-acetyl-gamma-butyrolactone, sodium bicarbonate and water as starting materials, chlorine gas is introduced for reaction, standing and layering are carried out after the reaction is finished, the product alpha-chloro-alpha-acetyl-gamma-butyrolactone can be obtained, the yield of the layering method is only 95%, and about 5% of the product in the remaining layering water can not be obtained and used. The loss of the α -chloro- α -acetyl- γ -butyrolactone product is about 0.365 tons per day, calculated as 5.76 tons of the raw material α -acetyl- γ -butyrolactone, while the unit price per ton of α -chloro- α -acetyl- γ -butyrolactone product is about 5.5 ten thousand yuan, corresponding to a loss of about 602.25 ten thousand yuan per year (calculated as 300 days of production). The reaction formula of the alpha-chloro-alpha-acetyl-gamma-butyrolactone synthesis process is as follows:
in addition, if the stratified water obtained here is treated as wastewater, the stratified water enters a three-effect system of a company environmental protection facility for distillation and desalination, however, due to the existence of the alpha-chloro-alpha-acetyl-gamma-butyrolactone in the stratified water, more viscous residues are generated in the distillation process, so that the normal operation of the company environmental protection facility is seriously influenced, and the efficiency of the company wastewater treatment is restricted.
If the organic solvent is used for extracting and recovering the alpha-chloro-alpha-acetyl-gamma-butyrolactone in the stratified water, the recovery of the organic solvent is difficult, new environmental pollution is caused, the VOC (volatile organic compounds) in tail gas is too high, and the treatment cost is high, so that the organic solvent is not suitable for extracting and recovering the alpha-chloro-alpha-acetyl-gamma-butyrolactone.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a method for recovering alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water, which can simply and efficiently recover residual alpha-chloro-alpha-acetyl-gamma-butyrolactone products in the stratified water, thereby forming economic benefits.
The invention also aims to provide the application of the method for recovering the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water in the synthesis of vitamin B1.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the invention provides a method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone, which comprises the following steps:
neutralizing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
Further, the recovery method comprises the following steps:
reducing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone, neutralizing the layered water with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
Further, the preparation method of the alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water comprises the following steps:
mixing alpha-acetyl-gamma-butyrolactone, water and an alkaline reagent, performing chlorination reaction, standing and layering to obtain alpha-chloro-alpha-acetyl-gamma-butyrolactone and alpha-chloro-alpha-acetyl-gamma-butyrolactone layering water;
further preferably, the alkaline agent comprises sodium bicarbonate.
Further, the reduction treatment includes at least one of treatment with a reducing agent and ultraviolet irradiation treatment.
Further, the reducing agent comprises at least one of sodium thiosulfate and sodium sulfite;
further preferably, the illumination time of the ultraviolet light irradiation treatment is 1-3 h;
further preferably, the ultraviolet light treatment comprises an ultraviolet sealing light treatment.
Further, the alkali includes at least one of sodium bicarbonate and calcium oxide.
Further, the method of evaporating moisture includes reduced pressure evaporation.
Furthermore, the vacuum degree of the reduced pressure evaporation is more than 0.095 Mpa;
further preferably, the temperature of the reduced pressure evaporation is 50-60 ℃.
Further, the recovery method comprises the following steps:
(a) mixing alpha-acetyl-gamma-butyrolactone, water and sodium bicarbonate, performing chlorination reaction, standing and layering to obtain alpha-chloro-alpha-acetyl-gamma-butyrolactone and alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water;
(b) neutralizing alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water with sodium bicarbonate, and evaporating water at 50 ℃ under vacuum of-0.095 Mpa to obtain recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone;
or, the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water is firstly reduced by sodium thiosulfate, neutralized by sodium bicarbonate and evaporated under vacuum of-0.095 Mpa and at 50 ℃ to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone;
or, the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is firstly reduced under ultraviolet sealed illumination, then neutralized by sodium bicarbonate, and then the water is evaporated under vacuum of-0.095 Mpa and at the temperature of 50 ℃, so as to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
In a second aspect, the present invention provides the use of a recovery process as described in any one of the preceding aspects for the synthesis of vitamin B1.
Compared with the prior art, the invention has at least the following beneficial effects:
the method for recovering the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water can simply and efficiently recover the alpha-chloro-alpha-acetyl-gamma-butyrolactone product remained in the stratified water, changes waste into valuable and forms economic benefit; meanwhile, the problem that the environment-friendly facility is not smooth to operate due to the fact that the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water is used as viscous substances generated in the process of carrying out distillation desalting on the wastewater is solved, and the operation efficiency of the environment-friendly facility is improved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to a first aspect of the present invention, there is provided a process for the recovery of α -chloro- α -acetyl- γ -butyrolactone stratified water, comprising the steps of:
neutralizing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
The recovery method can simply and efficiently recover the alpha-chloro-alpha-acetyl-gamma-butyrolactone product remained in the stratified water, changes waste into valuable and forms economic benefit; meanwhile, the problem that the environment-friendly facility is not smooth to operate due to viscous substances generated when the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water is used as wastewater for distillation and desalination is solved, and the operation efficiency of the environment-friendly facility is improved.
In a preferred embodiment, the recovery process of the present invention comprises the steps of:
reducing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone, neutralizing the layered water with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
The alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water is obtained by the following method, and comprises the following steps:
mixing alpha-acetyl-gamma-butyrolactone, water and an alkaline reagent, performing chlorination reaction, standing and layering to obtain alpha-chloro-alpha-acetyl-gamma-butyrolactone and alpha-chloro-alpha-acetyl-gamma-butyrolactone layering water;
among them, the alkaline agent includes, but is not limited to, sodium bicarbonate.
Because the alpha-chloro-alpha-acetyl-gamma-butyrolactone is obtained by reacting the alpha-acetyl-gamma-butyrolactone with chlorine in an alkaline aqueous solution, strong oxidizing substances exist in layered water obtained by standing and layering after the reaction is finished, and the recovery rate of products is influenced, so that the strong oxidizing substances in the layered water need to be treated, namely reduction treatment, then the layered water is neutralized by alkali, then water is evaporated, the alpha-chloro-alpha-acetyl-gamma-butyrolactone in the layered water is recovered, and the recovery rate can be further improved.
In the present invention, the reduction treatment includes at least one of treatment with a reducing agent and ultraviolet irradiation treatment; the reducing agent used in the present invention includes, but is not limited to, at least one of sodium thiosulfate and sodium sulfite; the ultraviolet light treatment of the present invention includes, but is not limited to, ultraviolet sealing light treatment, which can treat strongly oxidizing substances more efficiently and improve the recovery rate of the product than reducing agent treatment, and the light time of the ultraviolet light treatment of the present invention is 1 to 3 hours, and typical but not limiting light time is, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours.
In the invention, after strong oxide substances in the layered water are treated, alkali is needed to neutralize the layered water, and then water is evaporated to obtain a recovered product. Wherein, the alkali for neutralizing the stratified water in the present invention includes but is not limited to at least one of sodium bicarbonate (baking soda) and calcium oxide; the method for evaporating water in the invention includes, but is not limited to, reduced pressure evaporation, wherein the vacuum degree of the reduced pressure evaporation is above 0.095Mpa, and typical but not limiting reduced pressure evaporation vacuum degrees are, for example, 0.095Mpa, 0.096Mpa, 0.097Mpa, 0.098 Mpa; the temperature of reduced pressure evaporation in the present invention is 50 to 60 ℃, and typical but not limiting examples thereof are 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃ and 60 ℃.
In a preferred embodiment, the recovery process of the present invention comprises the steps of:
(a) mixing alpha-acetyl-gamma-butyrolactone, water and sodium bicarbonate, performing chlorination reaction, standing and layering to obtain alpha-chloro-alpha-acetyl-gamma-butyrolactone and alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water;
(b) neutralizing alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water with sodium bicarbonate, and evaporating water at 50 ℃ under vacuum of-0.095 Mpa to obtain recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone;
or, the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water is firstly reduced by sodium thiosulfate, neutralized by sodium bicarbonate and evaporated under vacuum of-0.095 Mpa and at 50 ℃ to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone;
or, the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is firstly reduced under ultraviolet sealed illumination, then neutralized by sodium bicarbonate, and then the water is evaporated under vacuum of-0.095 Mpa and at the temperature of 50 ℃, so as to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
The method can simply and efficiently recover the alpha-chloro-alpha-acetyl-gamma-butyrolactone from the stratified water by carrying out reduction treatment, alkali neutralization, reduced pressure evaporation and other operations on the stratified water, improves the economic benefit, solves the problem that the operation of the environmental protection facility is not smooth due to viscous substances generated when the stratified water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is used as wastewater for distillation and desalination treatment, and improves the technical effect of the operation efficiency of the environmental protection facility.
According to a second aspect of the invention, there is provided the use of a process for the recovery of layered water from α -chloro- α -acetyl- γ -butyrolactone for the synthesis of vitamin B1.
The invention is further illustrated by the following examples. The materials in the examples are prepared according to known methods or are directly commercially available, unless otherwise specified.
Example 1
(a) 192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.2g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 377.8g of layered water;
(b) the obtained stratified water was adjusted to neutral with 10g of sodium bicarbonate, and then distilled at a constant temperature of 50 ℃ under vacuum of-0.095 Mpa or more to obtain 11g of a product, water was detected as 70%, and only the peak pattern of α -chloro- α -acetyl- γ -butyrolactone was detected by weather, from which 3.3g of α -chloro- α -acetyl- γ -butyrolactone was recovered.
Example 2
(a) 192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.6g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 377.1g of layered water;
(b) the obtained layered water is firstly treated by adding 10g of sodium thiosulfate, then is adjusted to be neutral by 7.1g of baking soda, and then is steamed under the conditions of vacuum over 0.095Mpa and constant temperature of 50 ℃ to obtain 20g of product, the water content is detected to be 62%, only the peak type of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is detected by meteorology, and 7.6g of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is recovered.
Example 3
(a) 192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.5g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 377.2g of layered water;
(b) the obtained layered water is sealed and irradiated by ultraviolet rays for 1 hour, then is adjusted to be neutral by 9.5g of baking soda, and then is steamed under the conditions that the vacuum is controlled to be more than 0.095Mpa and the constant temperature is 50 ℃, so that 19g of a product is obtained, the water content is detected to be 47%, only the peak type of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is detected by weather, and 10.07g of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is obtained by recycling.
Example 4
(a) 192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.6g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 377.1g of layered water;
(b) the obtained layered water is sealed and irradiated by ultraviolet rays for 2 hours, then is adjusted to be neutral by 10.1g of baking soda, and then is steamed under the conditions that the vacuum is controlled to be more than 0.095Mpa and the constant temperature is 50 ℃, so that 17.2g of a product is obtained, the water content is detected to be 42 percent, only the peak type of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is detected by meteorology, and 9.97g of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is obtained by recycling.
Example 5
(a) 192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.5g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 376.9g of layered water;
(b) the obtained layered water is sealed and irradiated by ultraviolet rays for 3 hours, then is adjusted to be neutral by 9.5g of baking soda, and then is steamed under the conditions that the vacuum is controlled to be more than 0.095Mpa and the constant temperature is 50 ℃, so that 21.1g of a product is obtained, the water content is detected to be 44%, only the peak type of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is detected by weather, and 10.15g of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is recovered.
Comparative example 1
192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.4g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 377.6g of layered water;
the obtained layered water is not treated at all, and the yield of the product is only 95 percent.
Comparative example 2
(a) 192g of alpha-acetyl-gamma-butyrolactone, 125g of baking soda and 252g of water are put into reaction equipment, the temperature is controlled within 18 ℃, then 110g of chlorine is introduced for reaction, and after the reaction is finished, the mixture is kept stand for layering to obtain 231.4g of the product alpha-chloro-alpha-acetyl-gamma-butyrolactone and 377.6g of layered water;
(b) and extracting the obtained layered water with dichloromethane for three times, extracting with 50g of dichloromethane each time, combining the extract liquids, recovering 110g of dichloromethane, and recovering 9.8g of a product alpha-chloro-alpha-acetyl-gamma-butyrolactone.
The data for examples 1-5 and comparative examples 1-2 are shown in Table 1.
TABLE 1
As is apparent from Table 1, the recovered product, α -chloro- α -acetyl- γ -butyrolactone obtained by evaporating moisture after the reducing agent treatment or ultraviolet light treatment and alkali neutralization in examples 1 to 5 of the present invention, was high in yield and free from contamination, as compared with the methods of comparative examples 1 and 2.
The method recovers the alpha-chloro-alpha-acetyl-gamma-butyrolactone product from the layered water, has high yield, does not produce pollution, can generate the income of about 600 ten thousand yuan each year, thoroughly solves the problem that the environment-friendly facility is not smooth to operate due to viscous substances generated when the alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water is used as wastewater for distillation and desalination treatment, and improves the operation efficiency of the environment-friendly facility.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The method for recovering the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is characterized by comprising the following steps of:
neutralizing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
2. A recycling method according to claim 1, characterized in that it comprises the following steps:
reducing the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone, neutralizing the layered water with alkali, and evaporating water to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
3. The recovery process according to claim 1 or 2, characterized in that the preparation process of the α -chloro- α -acetyl- γ -butyrolactone stratified water comprises the following steps:
mixing alpha-acetyl-gamma-butyrolactone, water and an alkaline reagent, performing chlorination reaction, standing and layering to obtain alpha-chloro-alpha-acetyl-gamma-butyrolactone and alpha-chloro-alpha-acetyl-gamma-butyrolactone layering water;
preferably, the alkaline agent comprises sodium bicarbonate.
4. The recycling method according to claim 2, wherein the reduction treatment includes at least one of treatment with a reducing agent and ultraviolet irradiation treatment.
5. The recovery method according to claim 4, wherein the reducing agent includes at least one of sodium thiosulfate and sodium sulfite;
preferably, the illumination time of the ultraviolet light irradiation treatment is 1-3 h;
preferably, the ultraviolet light treatment comprises an ultraviolet sealing light treatment.
6. The recovery process of claim 1 or 2, wherein the base comprises at least one of sodium bicarbonate and calcium oxide.
7. A recovery process according to claim 1 or 2, characterized in that the process of evaporating moisture comprises reduced pressure evaporation.
8. The recovery method according to claim 7, wherein the degree of vacuum of the reduced pressure evaporation is 0.095Mpa or more;
preferably, the temperature of the reduced pressure evaporation is 50-60 ℃.
9. A recycling method according to claim 8, characterized in that it comprises the following steps:
(a) mixing alpha-acetyl-gamma-butyrolactone, water and sodium bicarbonate, performing chlorination reaction, standing and layering to obtain alpha-chloro-alpha-acetyl-gamma-butyrolactone and alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water;
(b) neutralizing alpha-chloro-alpha-acetyl-gamma-butyrolactone layered water with sodium bicarbonate, and evaporating water at 50 ℃ under vacuum of-0.095 Mpa to obtain recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone;
or, the alpha-chloro-alpha-acetyl-gamma-butyrolactone stratified water is firstly reduced by sodium thiosulfate, neutralized by sodium bicarbonate and evaporated under vacuum of-0.095 Mpa and at 50 ℃ to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone;
or, the layered water of the alpha-chloro-alpha-acetyl-gamma-butyrolactone is firstly reduced under ultraviolet sealed illumination, then neutralized by sodium bicarbonate, and then the water is evaporated under vacuum of-0.095 Mpa and at the temperature of 50 ℃, so as to obtain the recovered alpha-chloro-alpha-acetyl-gamma-butyrolactone.
10. Use of the recovery process of any one of claims 1-9 in the synthesis of vitamin B1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111622812.6A CN114181178A (en) | 2021-12-28 | 2021-12-28 | Method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111622812.6A CN114181178A (en) | 2021-12-28 | 2021-12-28 | Method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114181178A true CN114181178A (en) | 2022-03-15 |
Family
ID=80606222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111622812.6A Pending CN114181178A (en) | 2021-12-28 | 2021-12-28 | Method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114181178A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115850211A (en) * | 2022-11-29 | 2023-03-28 | 江苏兄弟维生素有限公司 | Process method for synthesizing and coproducing acetamidine hydrochloride from alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
| CN115925655A (en) * | 2022-11-29 | 2023-04-07 | 江苏兄弟维生素有限公司 | Process method for synthesizing and co-producing sodium bicarbonate solution by alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000355588A (en) * | 1999-06-10 | 2000-12-26 | Daicel Chem Ind Ltd | Production of alfa-acetyl-gamma-butyrolactone |
| JP2002173489A (en) * | 2000-12-05 | 2002-06-21 | Daicel Chem Ind Ltd | METHOD FOR PRODUCING alpha-ACETYL-gamma-BUTYLOLACTONE |
| EP1375490A1 (en) * | 2002-06-25 | 2004-01-02 | Degussa AG | Process for the production of 2-acetyl-2-chloro-gamma-butyrolactone |
| CN103387557A (en) * | 2012-05-08 | 2013-11-13 | 江苏兄弟维生素有限公司 | Continuous synthesis process of alpha-chloro-alpha-acetyl-gamma-butyrolactone |
| CN111018811A (en) * | 2019-12-20 | 2020-04-17 | 江西天新药业股份有限公司 | Method for preparing α -chloro- α -acetyl-gamma-butyrolactone |
| CN111018812A (en) * | 2019-12-27 | 2020-04-17 | 江苏兄弟维生素有限公司 | Process for chlorinating esters and process for separating chloroesters |
| CN112321543A (en) * | 2020-10-29 | 2021-02-05 | 安徽圣诺贝化学科技有限公司 | Preparation method of alpha-chloro-alpha acetyl-gamma-butyrolactone |
-
2021
- 2021-12-28 CN CN202111622812.6A patent/CN114181178A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000355588A (en) * | 1999-06-10 | 2000-12-26 | Daicel Chem Ind Ltd | Production of alfa-acetyl-gamma-butyrolactone |
| JP2002173489A (en) * | 2000-12-05 | 2002-06-21 | Daicel Chem Ind Ltd | METHOD FOR PRODUCING alpha-ACETYL-gamma-BUTYLOLACTONE |
| CN1357545A (en) * | 2000-12-05 | 2002-07-10 | 大赛璐化学工业株式会社 | Prepn of alpha-acetyl-gamma butyrolactone |
| EP1375490A1 (en) * | 2002-06-25 | 2004-01-02 | Degussa AG | Process for the production of 2-acetyl-2-chloro-gamma-butyrolactone |
| CN103387557A (en) * | 2012-05-08 | 2013-11-13 | 江苏兄弟维生素有限公司 | Continuous synthesis process of alpha-chloro-alpha-acetyl-gamma-butyrolactone |
| CN111018811A (en) * | 2019-12-20 | 2020-04-17 | 江西天新药业股份有限公司 | Method for preparing α -chloro- α -acetyl-gamma-butyrolactone |
| CN111018812A (en) * | 2019-12-27 | 2020-04-17 | 江苏兄弟维生素有限公司 | Process for chlorinating esters and process for separating chloroesters |
| CN112321543A (en) * | 2020-10-29 | 2021-02-05 | 安徽圣诺贝化学科技有限公司 | Preparation method of alpha-chloro-alpha acetyl-gamma-butyrolactone |
Non-Patent Citations (1)
| Title |
|---|
| 张莉: "α-乙酰基-γ-丁内酯的合成及进展", 《湖北化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115850211A (en) * | 2022-11-29 | 2023-03-28 | 江苏兄弟维生素有限公司 | Process method for synthesizing and coproducing acetamidine hydrochloride from alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
| CN115925655A (en) * | 2022-11-29 | 2023-04-07 | 江苏兄弟维生素有限公司 | Process method for synthesizing and co-producing sodium bicarbonate solution by alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114181178A (en) | Method for recovering layered water of alpha-chloro-alpha-acetyl-gamma-butyrolactone and application thereof | |
| CN100519497C (en) | Method for extraction separation of dichloropropanol from dichloropropanol hydrochloric water solution | |
| KR20100051104A (en) | Process and apparatus for purification of industrial brine | |
| CN214399818U (en) | Device for purifying hydrogen chloride by calcium chloride method containing impurity dilute hydrochloric acid | |
| CN102952101A (en) | Process for producing epoxypropane by adopting caustic soda saponification method | |
| CN111333842A (en) | Synthesis method of hydroxyl silicone oil | |
| CN100489012C (en) | Polymerizing solution reusing method for polymerization of paraphthaolyl p-phenylenediamine | |
| CN105714129B (en) | Comprehensive treatment method for extraction stage in cobalt hydrometallurgy | |
| CN113120925B (en) | Method for recovering iodide from isophorone cracking material | |
| CN108017233B (en) | Method for treating sewage of forestry chemical enterprises | |
| CN110422955B (en) | Resource recycling method for hazardous waste acid by using reaction heat | |
| CN110902696A (en) | Preparation method of cyanogen chloride | |
| CN105947984A (en) | Production process for recycling and producing anhydrous hydrogen fluoride from high-concentration wastewater containing fluoride | |
| CN115057784A (en) | Method for treating octyl trichlamide wastewater | |
| CN110845651B (en) | Process for improving bromine utilization rate in brominated butyl rubber | |
| CN109368859B (en) | Zero-discharge treatment process for fluoride-applying wastewater in steroid drug production | |
| CN111072053B (en) | Method for treating raffinate in recovery process of para-aramid solvent | |
| CN111362888B (en) | Production method and production system for propylene oxide by caustic soda saponification method | |
| CN1185434A (en) | Extraction method for hydroperoxide | |
| KR102197931B1 (en) | Method for manufacturing carbonate in a row and seawater pretreatment method to reduce scale of desalination plant | |
| CN103435441B (en) | The method of dimethyl malonate production wastewater treatment and resource reclaim | |
| CN109369339B (en) | Method for treating waste p-toluenesulfonic acid iron n-butanol solution | |
| CN106365951A (en) | 2-bromopropane recycling and reuse process in preparation process of 2,2-Diisopropylpropionitrile | |
| CN112919678A (en) | Acetic acid production wastewater treatment process | |
| CN108218075B (en) | Method for recovering organic matters from waste liquid generated in production of methane chloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220315 |
|
| RJ01 | Rejection of invention patent application after publication |