CN105198781A - Method of treating solid waste produced in beta-mercaptopropionic acid production process - Google Patents
Method of treating solid waste produced in beta-mercaptopropionic acid production process Download PDFInfo
- Publication number
- CN105198781A CN105198781A CN201510569326.0A CN201510569326A CN105198781A CN 105198781 A CN105198781 A CN 105198781A CN 201510569326 A CN201510569326 A CN 201510569326A CN 105198781 A CN105198781 A CN 105198781A
- Authority
- CN
- China
- Prior art keywords
- filter cake
- mercaptopropionic acid
- production process
- solid waste
- acid production
- 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.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method of treating solid waste produced in a beta-mercaptopropionic acid production process. The solid waste produced in the beta-mercaptopropionic acid production process is used as a raw material to be washed, press filtered, secondarily re-crystallized, vacuum filtered, dried and crushed to obtain 3,3'-thiodipropionic acid (TDPA) having an antioxidant function. The method has the beneficial effects that the solid waste produced in the betal-mercaptopropionic acid production process is converted to the non-toxic antioxidant TDPA by virtue of a re-crystallization process, so that the pollution of the solid waste in the beta-mercaptopropionic acid production process on the environment is avoided, and the adopted process discharges no waste water and is environment-friendly; the converted antioxidant TDPA is wide in industrial application, and the waste is converted into treasure, and the economic benefit produced by the beta- mercaptopropionic acid is increased.
Description
Technical field
The present invention relates to field of fine chemical, the treatment process of the solid waste produced in β-mercaptopropionic acid production process specifically.
Background technology
β-mercaptopropionic acid is produced with acrylonitrile process, there are the advantages such as operating procedure is simple, product yield is high, quality is high, but because β-mercaptopropionic acid is with the higher mercapto groups of reactive behavior, inevitably there is side reaction in process of production and form solid waste, through high resolution mass spectrum analysis, in the solid waste of formation, main component is sulfide compound.From the viewpoint of environmental protection, solid waste becomes increasingly conspicuous to the production of people, the infringement problem caused of living, therefore explore a kind of fixed-end forces method in β-mercaptopropionic acid production process, and be translated into nontoxic antioxidant thio-2 acid (TDPA) and have very important meaning.
Summary of the invention
The technical problem that the present invention mainly solves the by product produced in β-mercaptopropionic acid production process is converted into a kind of nontoxic antioxidant thio-2 acid (TDPA), and its structure is: S(CH
2cH
2cOOH)
2.
The treatment process of the solid waste produced in β-mercaptopropionic acid production process of the present invention is with the solid waste produced in β-mercaptopropionic acid production process for raw material, obtains the thio-2 acid (TDPA) with antioxygenation by washing, press filtration, secondary recrystallization, vacuum filtration, drying, pulverizing.
A treatment process for the solid waste produced in β-mercaptopropionic acid production process, is characterized in that: comprise the following steps:
A) solid waste produced in β-mercaptopropionic acid production process is put into enamel still, the weight ratio according to 1:1.5 ~ 2 adds deionized water, opens and stirs, and stirs 20 ~ 30min, stops stirring;
B) the product press filtration will a) obtained, during filtrate recycle is produced to β-mercaptopropionic acid, filter cake is collected pending;
C) proceed in enamel reaction still by filter cake b) obtained, the weight ratio according to 1:0.5 ~ 0.7 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
D) backflow terminate after, by phegma heat filtering, filtrate collection in strumbox, naturally cooling;
E) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
F) proceed in enamel reaction still by filter cake e) obtained, the weight ratio according to 1:0.5 ~ 0.7 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
G), after backflow terminates, by phegma heat filtering, filtrate collection is in strumbox, and naturally cooling, carries out secondary recrystallization;
H) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
I) the filter cake S(CH (h) obtained
2cH
2cOOH)
2saturated solution washing, vacuum filtration, filtrate recycles and reuses, filter cake collect pending;
J) filter cake (i) obtained is put into drying room, dry 5 ~ 10h at 30 ~ 50 DEG C;
K) solid (j) obtained is pulverized, and obtain target compound thio-2 acid (TDPA), its structural formula is as follows:
S（CH
2CH
2COOH）
2；
L) when after secondary precipitation flakes solid in (e), (h) filtrate, vacuum filtration, filtrate collection is in enamel reaction still, and logical steam heating distillation, reclaims dehydrated alcohol at 80 ~ 90 DEG C, and filter cake carries out crystallization again according to (f), (g) operation.
Target product is detected by nucleus magnetic resonance, and determines fusing point.
The present invention is the strict consumption controlling deionized water in treating processes, water soluble component in solid waste is dissolved in a large number, ensure to want the thio-2 acid of recrystallization (TDPA) crude product to have higher purity, accelerate recrystallization speed, simultaneously washing after water soluble liq as a supplement Water circulation to β-mercaptopropionic acid produce in, non-wastewater discharge; Organic solvent is selected to carry out recrystallization to crude product in invention, because inorganic salt are almost insoluble in organic solvent, the content of inorganic salt in product is dropped to minimum, strictly controls the usage quantity of recrystallization solvent simultaneously, target product can be crystallized out in the short period of time; In the present invention, secondary recrystallization is carried out to thio-2 acid (TDPA) crude product, ensure that the purity of thio-2 acid (TDPA); The present invention is by controlling the bake out temperature of thio-2 acid (TDPA), and prevent because temperature is too high, product is oxidized, and ensure that the quality of product; The recrystallization solvent simultaneously used in invention can pass through air distillation recycling, has saved production cost, has had higher economic benefit.
The present invention's beneficial effect is compared with prior art: by recrystallizing technology, the solid waste in β-mercaptopropionic acid production process is converted into a kind of nontoxic antioxidant thio-2 acid (TDPA), avoid the solid waste pollution on the environment in β-mercaptopropionic acid production process, the technique non-wastewater discharge that the present invention adopts, green, environmental protection; The antioxidant thio-2 acid (TDPA) transformed has industrial use widely, turns waste into wealth, and improves the economic benefit that β-mercaptopropionic acid is produced.
Embodiment
Embodiment 1
The treatment process of the solid waste produced in β-mercaptopropionic acid production process, comprises the following steps:
A) the solid waste 300kg produced in β-mercaptopropionic acid production process is added in 1000L enamel still, add 450kg deionized water, open and stir, stir 30min, stop stirring;
B) the product press filtration will a) obtained, during filtrate recycle is produced to β-mercaptopropionic acid, filter cake is collected pending;
C) proceed in 1000L enamel reaction still by filter cake b) obtained, the weight ratio according to 1:0.5 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
D) backflow terminate after, by phegma heat filtering, filtrate collection in 500L strumbox, naturally cooling;
E) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to 500L strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
F) proceed in 1000L enamel reaction still by the filter cake that (e) obtains, the weight ratio according to 1:0.5 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
G), after backflow terminates, by phegma heat filtering, filtrate collection is in 500L strumbox, and naturally cooling, carries out secondary recrystallization;
H) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to 500L strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
I) the filter cake S(CH (h) obtained
2cH
2cOOH)
2the washing of saturated ethanolic soln, vacuum filtration, filtrate recycles and reuses, and filter cake is collected pending;
J) filter cake (i) obtained is put into drying room, dry 5h at 50 DEG C;
K) solid (j) obtained is pulverized, and obtain target compound thio-2 acid (TDPA), its structural formula is as follows:
S（CH
2CH
2COOH）
2；
L) when after secondary precipitation flakes solid in (e), (h) filtrate, vacuum filtration, filtrate collection is in 1000L enamel reaction still, and logical steam heating distillation, reclaims dehydrated alcohol at 85 DEG C.Filter cake carries out secondary recrystallization according to (f), (g) operation;
Product yield is 78%; The target compound purity by magnetic resonance detection, inclusion-free peak on spectrogram, target compound purity is 100%; Simultaneously test target chemical combination fusing point, melting range is 132 ~ 133 DEG C.
Embodiment 2
The treatment process of the solid waste produced in β-mercaptopropionic acid production process, comprises the following steps:
A) the solid waste 300kg produced in β-mercaptopropionic acid production process is added in 1000L enamel still, add 600kg deionized water, open and stir, stir 20min, stop stirring;
B) the product press filtration will a) obtained, during filtrate recycle is produced to β-mercaptopropionic acid, filter cake is collected pending;
C) proceed in 1000L enamel reaction still by filter cake b) obtained, the weight ratio according to 1:0.7 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
D) backflow terminate after, by phegma heat filtering, filtrate collection in 500L strumbox, naturally cooling;
E) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to 500L strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
F) proceed in 1000L enamel reaction still by the filter cake that (e) obtains, the weight ratio according to 1:0.7 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
G), after backflow terminates, by phegma heat filtering, filtrate collection is in 500L strumbox, and naturally cooling, carries out secondary recrystallization;
H) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to 500L strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
I) the filter cake S(CH (h) obtained
2cH
2cOOH)
2saturated solution washing, vacuum filtration, filtrate recycles and reuses, filter cake collect pending;
J) filter cake (i) obtained is put into drying room, dry 8h at 40 DEG C;
K) solid (j) obtained is pulverized, and obtain target compound thio-2 acid (TDPA), its structural formula is as follows:
S（CH
2CH
2COOH）
2；
L) when after secondary precipitation flakes solid in (e), (h) filtrate, vacuum filtration, filtrate collection is in 1000L enamel reaction still, and logical steam heating distillation, reclaims dehydrated alcohol at 90 DEG C.Filter cake carries out secondary recrystallization according to (f), (g) operation;
Product yield is 65%; The target compound purity by magnetic resonance detection, inclusion-free peak on spectrogram, target compound purity is 100%; Simultaneously test target chemical combination fusing point, melting range is 132 ~ 133 DEG C.
Claims (1)
1. a treatment process for the solid waste produced in β-mercaptopropionic acid production process, is characterized in that: comprise the following steps:
A) solid waste produced in β-mercaptopropionic acid production process is put into enamel still, the weight ratio according to 1:1.5 ~ 2 adds deionized water, opens and stirs, and stirs 20 ~ 30min, stops stirring;
B) the product press filtration will a) obtained, during filtrate recycle is produced to β-mercaptopropionic acid, filter cake is collected pending;
C) proceed in enamel reaction still by filter cake b) obtained, the weight ratio according to 1:0.5 ~ 0.7 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
D) backflow terminate after, by phegma heat filtering, filtrate collection in strumbox, naturally cooling;
E) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
F) proceed in enamel reaction still by filter cake e) obtained, the weight ratio according to 1:0.5 ~ 0.7 adds dehydrated alcohol, opens and stirs, and leads to and is steam heated to 80 DEG C, backflow 2h;
G), after backflow terminates, by phegma heat filtering, filtrate collection is in strumbox, and naturally cooling, carries out secondary recrystallization;
H) after having a large amount of snowflake crystal to separate out in case to be filtered, vacuum filtration, place in filtrate collection to strumbox until no longer include snowflake crystal precipitation, filter cake is collected pending;
I) the filter cake S(CH (h) obtained
2cH
2cOOH)
2saturated solution washing, vacuum filtration, filtrate recycles and reuses, filter cake collect pending;
J) filter cake (i) obtained is put into drying room, dry 5 ~ 10h at 30 ~ 50 DEG C;
K) solid (j) obtained is pulverized, and obtain target compound thio-2 acid (TDPA), its structural formula is as follows:
S（CH
2CH
2COOH）
2；
L) when after secondary precipitation flakes solid in (e), (h) filtrate, vacuum filtration, filtrate collection is in enamel reaction still, and logical steam heating distillation, reclaims dehydrated alcohol at 80 ~ 90 DEG C, and filter cake carries out crystallization again according to (f), (g) operation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510569326.0A CN105198781B (en) | 2015-09-10 | 2015-09-10 | Method of treating solid waste produced in beta-mercaptopropionic acid production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510569326.0A CN105198781B (en) | 2015-09-10 | 2015-09-10 | Method of treating solid waste produced in beta-mercaptopropionic acid production process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105198781A true CN105198781A (en) | 2015-12-30 |
| CN105198781B CN105198781B (en) | 2017-05-24 |
Family
ID=54946782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510569326.0A Expired - Fee Related CN105198781B (en) | 2015-09-10 | 2015-09-10 | Method of treating solid waste produced in beta-mercaptopropionic acid production process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105198781B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02121962A (en) * | 1988-10-28 | 1990-05-09 | Daicel Chem Ind Ltd | Production of mercaptocarboxylic acid |
| CN1793117A (en) * | 2005-12-20 | 2006-06-28 | 顾建荣 | Preparation method of 3-mercaptopropionic acid |
| CN101125827A (en) * | 2007-09-18 | 2008-02-20 | 顾建荣 | Preparation method of 3-mercaptopropionic acid |
-
2015
- 2015-09-10 CN CN201510569326.0A patent/CN105198781B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02121962A (en) * | 1988-10-28 | 1990-05-09 | Daicel Chem Ind Ltd | Production of mercaptocarboxylic acid |
| CN1793117A (en) * | 2005-12-20 | 2006-06-28 | 顾建荣 | Preparation method of 3-mercaptopropionic acid |
| CN101125827A (en) * | 2007-09-18 | 2008-02-20 | 顾建荣 | Preparation method of 3-mercaptopropionic acid |
Non-Patent Citations (1)
| Title |
|---|
| 冯柏成: "β-巯基丙酸的合成研究", 《青岛化工学院学报》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105198781B (en) | 2017-05-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101168522B (en) | Method for preparing high purity lutein crystal from marigold oil resin | |
| CN101434566A (en) | Production process of methyl p-tolyl sulfone | |
| CN104003427A (en) | Method for preparing sheet high-purity lithium hydroxide by using spodumene concentrate | |
| WO2021068501A1 (en) | Method for synthesizing myricetin | |
| CN102675242A (en) | Refining method of vulkacit M | |
| CN112897599A (en) | Crystallization method of nickel sulfate, cobalt sulfate and manganese sulfate | |
| CN104529935B (en) | Method for synthesizing ethyl 2-(3-aldehyde-4-isobutyloxyphenyl)-4-methylthiazole-5-formate | |
| CN112300071B (en) | Synthetic method of high-purity chloroquine phosphate | |
| CN105198781A (en) | Method of treating solid waste produced in beta-mercaptopropionic acid production process | |
| CN103467252A (en) | Method for increasing purity of di-trimethylolpropane | |
| CN108675919A (en) | A kind of method that double trimethylolpropane is extracted in trimethylolpropane heavy constituent | |
| CN108147985B (en) | Preparation method of zinc dibutyl dithiocarbamate | |
| CN104945357A (en) | Refining method of dehydroandrographolide succinate | |
| CN102952074A (en) | Method of recycling dextromethorphan from crystallization mother liquor | |
| CN101284775B (en) | Process for reclaiming 2-keto-L-gulonate by salting out method | |
| CN109232222B (en) | Preparation method of (E) -octyl-4-ene-1, 8-diacid | |
| CN110066257B (en) | Purification method of 2-methyl-4-isothiazoline-3-ketone | |
| CN102731340A (en) | Preparation method of demethyl aureomycin hydrochloride | |
| CN108546232B (en) | Preparation method of mono-substituted or di-substituted benzoate compound | |
| CN113004168A (en) | Production process of methoxyamine for synthesizing furan ammonium salt | |
| CN112266329A (en) | Efficient production method of bromhexine hydrochloride | |
| CN111925355A (en) | Benzoselenophenol compound and preparation method thereof | |
| CN105502301B (en) | A kind of extracting method of sulfur waste sulphur cycling and reutilization | |
| CN106977509B (en) | The multiple water law method for crystallising of thiamine hydrochloride | |
| CN1683247A (en) | Process for producing anhydrous aluminium chloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170524 Termination date: 20210910 |