CN114229982A - Oxidation treatment device and method for AK sugar crystallization waste liquid - Google Patents
Oxidation treatment device and method for AK sugar crystallization waste liquid Download PDFInfo
- Publication number
- CN114229982A CN114229982A CN202111392938.9A CN202111392938A CN114229982A CN 114229982 A CN114229982 A CN 114229982A CN 202111392938 A CN202111392938 A CN 202111392938A CN 114229982 A CN114229982 A CN 114229982A
- Authority
- CN
- China
- Prior art keywords
- waste liquid
- sugar
- hydrogen peroxide
- crystallization waste
- storage tank
- 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.)
- Withdrawn
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
- B01J19/305—Supporting elements therefor, e.g. grids, perforated plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an AK sugar crystallization waste liquid oxidation treatment device and a method, which are characterized in that: the crystallization waste liquid storage tank and the hydrogen peroxide storage tank are respectively connected with a rapid mixer through pipelines, and the rapid mixer is sequentially connected with the tower reactor and the solution storage tank through pipelines; respectively pumping the primary crystallization waste liquid and hydrogen peroxide with the concentration of 10-55% into a rapid mixer for mixing, controlling the content of the added hydrogen peroxide to be 3-60% of the total volume concentration, then feeding the mixture into the top of a tower reactor, controlling the temperature of the tower reactor to be 0-100 ℃, and reacting for 1-240 min, feeding the liquid discharged from the tower reactor into a solution storage tank, and then applying the liquid to AK sugar production. The invention has the advantages that: the damage caused by local overheating and overpressure due to the generation of a large amount of gas and heat is avoided, and the process is efficient and safe; after the hydrogen peroxide treatment, the organic high molecular compound with dark color is oxidized into small molecules to be removed, so that a yellow clear solution is obtained, the material consumption can be reduced by recycling, and the quality of the recycled product is not influenced.
Description
Technical Field
The invention belongs to the technical field of acesulfame potassium production, and relates to an AK sugar crystallization waste liquid oxidation treatment device and method.
Background
AK sugar, also known as Acesulfame K, is called Potassium acetylsulfanilate, 6-methyl-2, 2-dioxo-1, 2, 3-oxathiaza-4-cyclohexenone Potassium salt, and Acesulfame Potassium (Acesulfame K), abbreviated as ASK. The method is used for producing the AK sugar by taking diketene, sulfamic acid, triethylamine and sulfur trioxide as main raw materials, has the advantages of easily obtained raw materials, mild reaction conditions, higher yield, low cost, good product quality and the like, and is adopted by most of AK sugar manufacturers at present. The production process comprises the following steps: (1) preparation of acetoacetamidosulfonate: suspending sulfamic acid and triethylamine in a solvent, and introducing diketene under the condition of controlling the temperature to obtain a nearly colorless solution; (2) preparation of a sulfur trioxide/dichloromethane solution: introducing sulfur trioxide into dichloromethane to obtain a solution; (3) preparation of AK sugar intermediate: cyclizing the acetoacetamidosulfonate solution with sulfur trioxide/dichloromethane solution at low temperature to obtain AK sugar intermediate; (4) preparation of AK sugar: and (3) hydrolyzing the AK sugar intermediate, extracting with dichloromethane, neutralizing the dichloromethane with potassium hydroxide for reaction, distilling off the dichloromethane, and decoloring, evaporating and crystallizing the water phase to obtain the AK sugar.
Generally, the primary crystallization mother liquor can be discharged as wastewater due to deep color, about 0.5 ton of wastewater is generated when 1 ton of AK sugar is produced, and the direct discharge can cause environmental pollution and increase the cost of the product, because the primary crystallization mother liquor contains 20-30% of potassium salt, mainly potassium carbonate, a small amount of potassium sulfamate, potassium sulfate and potassium hydroxide, 1-3% of AK sugar, and a small amount of organic high molecular compounds (mainly polymerized acetoacetic acid compounds), and the direct discharge of the strong alkaline crystallization mother liquor can cause environmental pollution and great economic loss.
Patent publication No. CN102336647B provides an application of AK sugar crystallization mother liquor and a method for preparing potassium salt by using the crystallization mother liquor, wherein the crystallization mother liquor is directly mixed with organic acid or inorganic acid, and a potassium salt product is prepared by cooling, filtering and recrystallizing; because the technical scheme does not consider the influence of components such as sulfamate, AK sugar byproducts and the like in the crystallization mother liquor, the purity of the obtained crude potassium salt product is not high, and a purer potassium salt product can be obtained only by recrystallization, while the residual waste liquor (containing components such as sulfamate, AK sugar byproducts and the like) after the original crystallization mother liquor is extracted with potassium salt needs to be treated, and meanwhile, secondary mother liquor/waste liquor is also generated by the recrystallization of impure potassium salt; therefore, the technology only utilizes potassium resources, does not solve the problem of organic impurities, and generates more secondary pollution.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides an AK sugar crystallization waste liquid oxidation treatment device and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an oxidation treatment device of AK sugar crystallization waste liquid is characterized by comprising the following equipment:
the crystallization waste liquid storage tank and the hydrogen peroxide storage tank are respectively connected with a rapid mixer through pipelines, and the rapid mixer is sequentially connected with the tower reactor and the solution storage tank through pipelines; wherein, metering pumps are respectively arranged on the pipelines among the crystallization waste liquid storage tank, the hydrogen peroxide storage tank and the rapid mixer.
Further, the rapid mixer is a microchannel reactor, a pipeline reactor or a rapid stirring reactor; the measured crystallization waste liquid and hydrogen peroxide can be quickly mixed in a quick mixer in a small amount, and the mixture enters a tower reactor after a quick oxidation reaction.
Further, the tower reactor is a packed tower, a plate tower, a packed plate tower (i.e., a tower equipped with both a plate and a packing) or a reaction tower with a downcomer.
Crystallization waste liquid and hydrogen peroxide solution pass through the flash mixer mixing reaction after, get into the top of tower reactor, because the oxidation that takes place in the mixing reactor should produce a large amount of heat and gas, and steam, and the reaction can last a period of time, therefore the reaction mixture flows downwards under the action of gravity from the top of tower reactor, can continue violent reaction at this in-process, and the gas and the steam that produce can be from down up discharge tower reactor, the heat that produces in this in-process can maintain longer thermal oxidation and take place, guarantee that the reaction goes on completely.
An oxidation treatment method of AK sugar crystallization waste liquid is characterized by comprising the following steps: respectively pumping primary crystallization waste liquid (1.0-20% of potassium carbonate, 0.1-5% of potassium sulfamate, 0.1-5% of potassium sulfate, 1.0-20% of potassium hydroxide and 0.1-5% of acesulfame potassium) and hydrogen peroxide (with the concentration of 10-55%) generated in the AK sugar production process into a rapid mixer for mixing, controlling the content of the added hydrogen peroxide to be 3-60% of the total volume concentration, then feeding the mixture into the top of a tower reactor, controlling the temperature of the tower reactor to be 0-100 ℃ and the reaction time to be 1-240 min, feeding liquid (potassium salt solution) discharged from the tower reactor into a solution storage tank, and then mechanically applying the liquid (potassium salt solution) to the AK sugar production (applied to the step of neutralizing hydrolysis extract phase and partially replacing potassium hydroxide for use).
Further, the content of the added hydrogen peroxide is 15-45% of the total volume concentration.
Further, the content of the added hydrogen peroxide is 20-30% of the total volume concentration.
Further, the temperature of the tower reactor is controlled to be 20-80 ℃, and the reaction time is 40-200 min.
Further, the temperature of the tower reactor is controlled to be 35-60 ℃, and the reaction time is 80-150 min.
Further, the application method of the potassium salt solution comprises the following steps: and (3) using the reacted potassium salt solution for neutralizing a dichloromethane solution in the AK sugar production process on the production line, dropwise adding the reacted potassium salt solution into the dichloromethane solution, and controlling the dropwise adding temperature to be-10-20 ℃.
The invention has the following advantages:
1. the device can effectively initiate and control violent oxidation reaction, avoid the harm caused by local overheating and overpressure formed by a large amount of generated gas and heat, ensure the production safety and efficiently carry out the process;
2. through mixing reaction of hydrogen peroxide and the primary crystallization waste liquid, organic components with deep color (possibly various macrocyclic conjugated ketones, such as documents J. org. chem., 1967, 32, 9, 2881-2887) in the primary crystallization waste liquid are fully oxidized, organic high molecular compounds with deep color are oxidized into small molecules such as carbon dioxide and the like and are removed, and a yellow clear solution (the color of an acesulfame potassium aqueous solution) is obtained;
3. the potassium salt solution treated by the hydrogen peroxide can replace potassium hydroxide to be recycled to the neutralization step of the hydrolysis extraction phase, so that the consumption of materials (potassium hydroxide) is reduced (the unit consumption is reduced from 0.7 ton/ton to 0.6 ton/ton), the production cost of AK sugar is reduced, the amount of discharged wastewater can be greatly reduced (from 3.0 ton/ton to 2.5 ton/ton), the potassium content in the wastewater is reduced (from 2% to below 0.2%), and the pollution of the wastewater to the environment is reduced;
4. the treated potassium salt solution can completely replace 40% potassium hydroxide solution used on a production line in the AK sugar production process, the obtained AK sugar crude product is almost the same as the original process, and the qualified acesulfame potassium product can be obtained after concentration, crystallization and purification. The result shows that the average yield of AK sugar after long-time cyclic utilization is improved by about 2%, the KOH consumption is reduced by about 15%, the production cost is reduced by about 3%, and the economic benefit is obvious.
Drawings
FIG. 1 is a schematic diagram of an apparatus for oxidation treatment of AK sugar crystallization waste liquid;
FIG. 2 is an HPLC chromatogram before and after oxidation treatment of the crystallization waste liquid.
Detailed Description
The invention is further illustrated with reference to fig. 1:
an oxidation treatment device of AK sugar crystallization waste liquid comprises the following equipment: the crystallization waste liquid storage tank (1) and the hydrogen peroxide storage tank (2) are respectively connected with a rapid mixer (5) through pipelines, and the rapid mixer is sequentially connected with a tower reactor (6) and a solution storage tank (7) through pipelines; wherein, metering pumps are respectively arranged on the pipelines among the crystallization waste liquid storage tank, the hydrogen peroxide storage tank and the rapid mixer.
An oxidation treatment method of AK sugar crystallization waste liquid comprises the following specific implementation steps:
example 1
100mL of primary crystallization waste liquid (10% of potassium carbonate, 2% of potassium sulfamate, 2.5% of potassium sulfate, 5% of potassium hydroxide and 2.5% of acesulfame potassium) generated in the AK sugar production process and 30mL of hydrogen peroxide (with the concentration of 50%) are respectively pumped into a rapid mixer (40 ℃) to be mixed (a large amount of bubbles and heat are generated after mixing), then the mixture enters the top of a tower reactor, along with the progress of reaction, a large amount of gas and heat are generated, the temperature in the tower reactor naturally rises to 90 ℃, the temperature is reduced to room temperature after reaction for 20min, the solution is changed into 130mL of bright yellow transparent solution (sylvite solution) (almost no organic component is detected by gas chromatography) from dark brown before the reaction, and the solution enters a solution storage tank for later use.
130mL of the bright yellow transparent solution obtained in the example 1 is dropwise added into a dichloromethane solution obtained after sulfonation cyclization hydrolysis in a 500mLAK sugar production process, bubbles are continuously generated, and the PH value is about 8-9 when at least bubbles are generated; adding a small amount of 40% potassium hydroxide until the pH value of the solution is 9-10, evaporating dichloromethane, decoloring with activated carbon, and evaporating for crystallization to obtain 70g of AK sugar crude product; the result shows that compared with the average yield of AK sugar primary sugar of 66-70 g, the yield is slightly improved after the crystallization waste liquid is applied.
Example 2
500mL of primary crystallization waste liquid (potassium carbonate 15%, potassium sulfamate 5%, potassium sulfate 3%, potassium hydroxide 8% and acesulfame-k 1%) generated in the AK sugar production process and 50mL of hydrogen peroxide (with the concentration of 50%) are respectively pumped into a rapid mixer (80 ℃) to be mixed (a large amount of bubbles and heat are generated after mixing), then the mixture enters the top of a tower reactor, along with the progress of reaction, a large amount of gas and heat are generated, the temperature in the tower reactor naturally rises to 100 ℃, the temperature is reduced to room temperature after reaction for 60min, the solution is changed into 550mL (almost no organic component is detected by gas chromatography) of bright yellow transparent solution (potassium salt solution) from dark brown before the reaction, and the solution enters a solution storage tank for later use.
Example 3
1000mL of primary crystallization waste liquid (potassium carbonate 20%, potassium sulfamate 1%, potassium sulfate 1%, potassium hydroxide 2% and acesulfame 5%) generated in the AK sugar production process and 200mL of hydrogen peroxide (with the concentration of 50%) are respectively pumped into a rapid mixer (10 ℃) to be mixed (a large amount of bubbles and heat are generated after mixing), then the mixture enters the top of a tower reactor, along with the progress of reaction, a large amount of gas and heat are generated, the temperature in the tower reactor naturally rises to 90 ℃, the temperature is reduced to room temperature after reaction for 20min, the solution is changed into 1200mL (almost no organic component is detected by gas chromatography) of bright yellow transparent solution (potassium salt solution) from dark brown before the reaction, and the solution enters a solution storage tank for later use.
Example 4
Respectively adding 1m of primary crystallization waste liquid (potassium carbonate 3%, potassium sulfamate 2%, potassium sulfate 3%, potassium hydroxide 8% and acesulfame potassium 4%) and hydrogen peroxide (concentration is 50%) generated in AK sugar production process3/h、0.2m3The reaction solution is pumped into a rapid mixer (10 ℃) for mixing (a large amount of bubbles and heat are generated after mixing), then enters the top of a tower reactor, along with the reaction, a large amount of gas and heat are generated, the temperature in the tower reactor naturally rises to 90 ℃, the temperature is reduced to room temperature after 40min of reaction, and the solution is changed into a bright yellow transparent solution (a potassium salt solution) 1.2m from dark brown before the reaction3And h (almost no organic components detected by gas chromatography) enters a solution storage tank for standby.
Claims (10)
1. An oxidation treatment device of AK sugar crystallization waste liquid is characterized by comprising the following equipment:
the crystallization waste liquid storage tank and the hydrogen peroxide storage tank are respectively connected with a rapid mixer through pipelines, and the rapid mixer is sequentially connected with the tower reactor and the solution storage tank through pipelines; wherein, metering pumps are respectively arranged on the pipelines among the crystallization waste liquid storage tank, the hydrogen peroxide storage tank and the rapid mixer.
2. The oxidation treatment device of AK sugar crystallization waste liquid according to claim 1, characterized in that: the rapid mixer is a microchannel reactor, a pipeline reactor or a rapid stirring reactor.
3. The apparatus for oxidation treatment of AK sugar crystallization waste liquid according to claim 1 or 2, characterized in that: the tower reactor is a packed tower, a plate tower, a packed plate tower or a reaction tower with a downcomer.
4. The method for oxidizing AK sugar crystallization waste liquid according to the device of claim 1, characterized by comprising the steps of: respectively pumping primary crystallization waste liquid generated in the AK sugar production process and hydrogen peroxide with the concentration of 10-55% into a rapid mixer for mixing, controlling the content of the added hydrogen peroxide to be 3-60% of the total volume concentration, then feeding the mixture into the top of a tower reactor, controlling the temperature of the tower reactor to be 0-100 ℃ and the reaction time to be 1-240 min, feeding liquid discharged from the tower reactor into a solution storage tank, and then mechanically applying the liquid to the AK sugar production.
5. The method for oxidation treatment of AK sugar crystallization waste liquid according to claim 4, characterized in that: 1.0-20% of potassium carbonate, 0.1-5% of potassium sulfamate, 0.1-5% of potassium sulfate, 1.0-20% of potassium hydroxide and 0.1-5% of acesulfame potassium are contained in the primary crystallization waste liquid; the concentration of the hydrogen peroxide is 10-35%.
6. The method for oxidation treatment of AK sugar crystallization waste liquid according to claim 4, characterized in that: the content of the added hydrogen peroxide is 10-45% of the total volume concentration.
7. The method for oxidation treatment of AK sugar crystallization waste liquid according to claim 4, characterized in that: the content of the added hydrogen peroxide is 20-30% of the total volume concentration.
8. The method for oxidation treatment of AK sugar crystallization waste liquid according to claim 4, characterized in that: the temperature of the tower reactor is controlled to be 20-80 ℃, and the reaction time is 40-200 min.
9. The method for oxidation treatment of AK sugar crystallization waste liquid according to claim 4, characterized in that: the temperature of the tower reactor is controlled to be 35-60 ℃, and the reaction time is 80-150 min.
10. The method for oxidation treatment of AK sugar crystallization waste liquid according to claim 4, characterized in that: the application method of the potassium salt solution comprises the following steps: and (3) using the reacted potassium salt solution for neutralizing a dichloromethane solution in the AK sugar production process on the production line, dropwise adding the reacted potassium salt solution into the dichloromethane solution, and controlling the dropwise adding temperature to be-10-20 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111392938.9A CN114229982A (en) | 2021-11-23 | 2021-11-23 | Oxidation treatment device and method for AK sugar crystallization waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111392938.9A CN114229982A (en) | 2021-11-23 | 2021-11-23 | Oxidation treatment device and method for AK sugar crystallization waste liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114229982A true CN114229982A (en) | 2022-03-25 |
Family
ID=80750532
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111392938.9A Withdrawn CN114229982A (en) | 2021-11-23 | 2021-11-23 | Oxidation treatment device and method for AK sugar crystallization waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114229982A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5744010A (en) * | 1992-03-17 | 1998-04-28 | Hoechst Aktiengesellschaft | Process for the preparation of the non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and arrangement for carrying out this process |
| CN102336647A (en) * | 2011-07-06 | 2012-02-01 | 滁州学院 | Application of AK sugar crystal mother liquor and method for preparing sylvite by crystal mother liquor |
| CN111377882A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN111518056A (en) * | 2020-05-23 | 2020-08-11 | 安徽金禾实业股份有限公司 | Treatment and utilization method of acesulfame potassium crystallization waste liquid |
| CN112194293A (en) * | 2020-09-26 | 2021-01-08 | 安徽金禾实业股份有限公司 | Recycling method of discharged mother liquor in acesulfame potassium production |
-
2021
- 2021-11-23 CN CN202111392938.9A patent/CN114229982A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5744010A (en) * | 1992-03-17 | 1998-04-28 | Hoechst Aktiengesellschaft | Process for the preparation of the non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and arrangement for carrying out this process |
| CN102336647A (en) * | 2011-07-06 | 2012-02-01 | 滁州学院 | Application of AK sugar crystal mother liquor and method for preparing sylvite by crystal mother liquor |
| CN111377882A (en) * | 2018-12-30 | 2020-07-07 | 南通醋酸化工股份有限公司 | Method for continuously producing acesulfame |
| CN111518056A (en) * | 2020-05-23 | 2020-08-11 | 安徽金禾实业股份有限公司 | Treatment and utilization method of acesulfame potassium crystallization waste liquid |
| CN112194293A (en) * | 2020-09-26 | 2021-01-08 | 安徽金禾实业股份有限公司 | Recycling method of discharged mother liquor in acesulfame potassium production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110330466B (en) | Method for recovering dibenzothiazyl disulfide from mother liquor of production of cephalosporin active ester | |
| CN111518056A (en) | Treatment and utilization method of acesulfame potassium crystallization waste liquid | |
| CN103613517B (en) | A kind of method preparing taurine | |
| CN114917848B (en) | Device and method for synthesizing vinyl sulfate | |
| CN109928872A (en) | A kind of method of high-purity synthesis anthraquinone co-producing sulfuric acid magnesium | |
| CN109503410A (en) | The method of solvent DMF recycling in a kind of production of Sucralose | |
| CN113912085A (en) | Production method of sodium bromide | |
| CN111116424B (en) | Method for preparing trifluoromethanesulfonic acid by continuous hydrolysis | |
| CN106496038A (en) | A kind of preparation method of 3 methyl, 2 nitrobenzoic acid of high selectivity | |
| CN114229982A (en) | Oxidation treatment device and method for AK sugar crystallization waste liquid | |
| CN102898328B (en) | Synthesis method of diethyl azodicarboxylate and intermediate of diethyl azodicarboxylate | |
| CN114133363A (en) | Method for recycling AK sugar from AK sugar crystallization waste liquid | |
| CN108164502B (en) | Preparation method of 1, 3-propane sultone | |
| CN114835611A (en) | Process and equipment for reducing content of sulfuric acid in sulfonated product heavy alkylbenzene sulfonic acid | |
| CN106243059A (en) | A kind of method extracting benzothiazole from 2 benzothiazolyl mercaptans production by-products | |
| CN101607871B (en) | Method for preparing 4,4' -dimethylolbiphenyl | |
| CN112961034B (en) | Clean naphthol production process taking sulfur trioxide as raw material | |
| CN110590509A (en) | Production method for carbon dioxide cyclic decomposition coking crude phenol coproduction desulfurizer | |
| CN107011216A (en) | A kind of preparation method of trans 4 Boc aminocyclohexane acetic acid | |
| RU2790161C1 (en) | Sodium bromide production method | |
| CN104356187B (en) | Method for recycling hydrocortisone in hydrocortisone butyrate mother liquor | |
| CN112979427B (en) | Process for synthesizing naphthol through sulfur trioxide indirect sulfonation reaction | |
| CN215049782U (en) | High-purity p-nitrochlorobenzene preparation system | |
| CN102898327A (en) | Synthesis method for dimethyl azodicarboxylate and intermediate thereof | |
| CN101723869A (en) | Method for improving synthesis process of isothiazolinone intermediate |
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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20220325 |
|
| WW01 | Invention patent application withdrawn after publication |