CN105502740B - A kind of method of material recycle in rubber antioxidant TMQ productions waste water - Google Patents
A kind of method of material recycle in rubber antioxidant TMQ productions waste water Download PDFInfo
- Publication number
- CN105502740B CN105502740B CN201510964282.1A CN201510964282A CN105502740B CN 105502740 B CN105502740 B CN 105502740B CN 201510964282 A CN201510964282 A CN 201510964282A CN 105502740 B CN105502740 B CN 105502740B
- Authority
- CN
- China
- Prior art keywords
- tmq
- waste water
- extractant
- floccule
- extraction
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
Abstract
The present invention relates to a kind of method that rubber antioxidant TMQ produces material recycle in waste water, by the waste water after neutralization after stratification, aqueous phase containing floccule adds extractant, stratification after extraction, aqueous phase is uniformly processed into sewage disposal system, and oil phase returns to reuse in batch condensation polymerization reactor.Extractant is aniline, TMQ synthons or Synthesis liquid；Raw materials used or building-up process intermediate mainly is synthesized from TMQ products, reaches the recycling of material inner loop.The present invention only needs in and divided after water using extractant extraction floccule, it is possible to reaches and removes pollutant, the low consumed purpose of drop, active principle recovery of extraction reaches more than 33%, and in floccule about 1/3rd active ingredient is all reclaimed.TMQ yields are improved, reduce Pollutants in Wastewater concentration, and reach consumption reduction, waste reduction, the purpose of environmental protection.Solves the process problem of TMQ saline sewages.
Description
Technical field
The invention belongs to age resistor TMQ production technical fields, thing in more particularly to a kind of rubber antioxidant TMQ productions waste water
Expect the method for recovery.
Background technology
It is anti-old that rubber antioxidant TMQ (RD, 2,2,4- trimethyl -1,2- dihyaroquinoline polymer) is mainly used as rubber
Agent, it is splendid to aging protection effect caused by heat and oxygen suitable for the rubber polymer such as natural gum and butyronitrile, butylbenzene, second third and neoprene.
All types of elastomers under various applicable cases are suitable for almost, temperature applicable range is wide.
It with aniline and acetone is reaction raw materials that currently used preparation method, which is, the polycondensation in the presence of acid catalyst, warp
Neutralize, distill, being molded, packing and produce TMQ finished products.Document (CN 103214640A) reports such a conjunction for preparing age resistor TMQ
Into technique.Need to remove catalyst by acid-base neutralization in TMQ production processes, generation neutralization waste water, waste water (water during this
Phase) end when discharging water is separated with material (oil phase), and per batch of material, all some floccule produces, it is difficult to be separated, if not
By this part discharge and stay in material can cause finished product ash content raise, influence final product quality, if discharge not only cause material
Waste and sewage disposal difficulty will be greatly promoted.Patent (CN 101353447A) reports one kind and uses solid acid catalysis
Age resistor TMQ synthesis technique is prepared, although the method can produce solid dangerous waste, intractability is big, simultaneously without neutralizing
TMQ effective contents are unstable in building-up process, therefore use range is small, do not promote completely, fail fundamentally solving environment dirt
Dye problem, traditional handicraft is taken substantially in TMQ production at home.
In traditional handicraft, the aqueous phase that feed separation goes out after waste water neutralizes is neutralized, as shown in figure 1, being directly discharged to sewage
Processing system, contain salt due to neutralizing in sewage, biochemical process can not be taken to handle sewage substantially；And containing in sewage largely has
Machine thing causes the method that can not take the desalinations such as distillation, because organic matter can cause line clogging to lead to not run；Its other party
Method is not very stable to the treatment effect of sewage, and operating cost is higher, thus the intractability of TMQ production waste water is very big.
For the present invention based on traditional handicraft, being conceived to reduces the content of organics neutralized in waste water, reduces sewage disposal
The thinking of difficulty, it is proposed that the method that recovery neutralizes floccule in waste water, in reducing sewage disposal difficulty and reclaiming sewage simultaneously
Utility, reduce product consumption.
The content of the invention
The main object of the present invention is to provide consumption reduction waste reduction new method in a kind of age resistor TMQ production processes, will prevent old
The floccule in waste water is neutralized in agent TMQ productions, active ingredient in floccule is recycled by extracting process, is extracted
Raw materials used or building-up process intermediate is synthesized from TMQ products, reaches the recycling of material inner loop, so as to reach
Consumption reduction, waste reduction, the purpose of environmental protection.
The present invention is achieved by the following technical solutions：
The method of material recycle, passes through stratification by the waste water after neutralization in a kind of rubber antioxidant TMQ productions waste water
Afterwards, aqueous phase containing floccule adds extractant, stratification after extraction, and aqueous phase is uniformly processed into sewage disposal system, and oil phase returns
Return to reuse in batch condensation polymerization reactor.
Described extractant with containing in floccule and the weight ratio of waste water is 1-20:1.
Described extractant is aniline, TMQ synthons or Synthesis liquid；Extractant is mainly from used in the synthesis of TMQ products
The intermediate of raw material or building-up process, reach the recycling of material inner loop.
Described extraction temperature is 30-95 DEG C.
Described extraction time is 0.5-2h.
The stratification time is 0.5-4h after described extraction.
Under conditions of stirring extractant is added to aqueous phase containing floccule.
By active principle in method floccule described above (monomer or two, three, the tetramer) recovery of extraction reaches
More than 33%, in floccule about 1/3rd active ingredient is all reclaimed.
The advantage of the invention is that：Only need in and divide after water using extractant extraction floccule, it is possible to reach and remove
Depollute thing, the low consumed purpose of drop, active principle reuse in floccule, improve TMQ yields, reduce Pollutants in Wastewater
Concentration, and reach consumption reduction, waste reduction, the purpose of environmental protection.Extractant is from raw material or middle product needed for reaction, without solvent recovery,
Direct reuse, it is simple, easy to operate, while solution recovery can be avoided to cause additionally to increase equipment and energy consumption.Reclaimed by floccule
Sewage afterwards can carry out desalting processing because organic matter is reduced after pretreatment, and desalter is without blocking, solution in processing procedure
Determine the process problems of TMQ saline sewages.
Brief description of the drawings
Fig. 1：It is directly discharged to sewage disposal system；
Fig. 2：The schematic flow sheet of the present invention.
Embodiment
Below by specific embodiment, the present invention is described in further detail：
The present invention is that the floccule extracting method in waste water is neutralized in a kind of age resistor TMQ production, as shown in Fig. 2 with
Extracted in device with stirring with extractant and neutralize floccule in waste water, stratification after extraction, aqueous phase enters sewage disposal
Systematic unity processing, the active principle extracted in oil phase (solvent phase) return in batch condensation polymerization reactor one and reacted reuse, pass through
Extraction extracts the floccule neutralized in waste water the yield of simultaneously reuse lifting TMQ productions, due to neutralizing sewage after extraction
Contained organic matter is reduced, therefore reduces intractability.
Following examples can make those skilled in the art that the present invention be more completely understood, but not limit this in any way
Invention.
Embodiment 1
By 100g containing (weight ratio is 1 with waste water (COD value 23000mg/L), 100g extractants aniline in floccule:1),
It is added in extraction kettle, stratification 0.5h, aqueous phase directly blow down to sewage disposal system after stirring extraction 0.5h at 30 DEG C,
Solvent phase (100.2g) is put into after metering synthesizes TMQ in batch condensation polymerization reactor, TMQ receipts amount, which more normally feeds intake, increases 0.25g；
COD value of waste water is reduced to 14500mg/L after extraction, while the smell of waste water reduces；After pretreatment, desalination can be carried out
Processing, to desalter without blocking；Extractant aniline is that reactant can be recycled directly, and loss amount is small, simple easily behaviour
Make, the feature of environmental protection is high.
Embodiment 2：
By 100g contain in floccule and waste water (COD value 23000mg/L), 200g extractant TMQ monomer liquids (weight ratio is
1:2), it is added in extraction kettle, the stratification 2h after stirring extraction 1h at 50 DEG C.Aqueous phase directly blow down to sewage disposal system
System, solvent phase (200.6g) is put into after metering synthesizes TMQ in batch condensation polymerization reactor, TMQ receipts amount more normally feeds intake increase
0.8g；COD value of waste water is reduced to 13500mg/L after extraction, while the smell of waste water reduces；After pretreatment, Ke Yijin
Row desalting processing, to desalter without blocking；Extractant TMQ monomers are reaction intermediate, can directly be recycled, loss
Measure small, simple to operation, feature of environmental protection height.
Embodiment 3：
By 100g contain floccule in and waste water (COD value 23000mg/L), 2000g extractant TMQ Synthesis liquid (weight ratios
For 1:20), it is added in extraction kettle, the stratification 4h after stirring extraction 2h at 95 DEG C.Aqueous phase directly blow down to sewage disposal
System, solvent phase (2001) is put into after metering synthesizes TMQ in batch condensation polymerization reactor, and TMQ receipts amount more normally feeds intake increase
0.6g, COD value of waste water is reduced to 15000mg/L after extraction, while the smell of waste water reduces；After pretreatment, Ke Yijin
Row desalting processing, to desalter without blocking；Extractant TMQ Synthesis liquids are reactant intermediate, can directly be recycled,
Loss amount is small, simple to operation, and the feature of environmental protection is high.
Embodiment 4：
By 100g contain in floccule and waste water (COD value 23000mg/L), 400g extractant TMQ monomer liquids (weight ratio is
1:4), it is added in extraction kettle, the stratification 3h after stirring extraction 2h at 50 DEG C.Aqueous phase directly blow down to sewage disposal system
System, solvent phase (400.5g) is put into after metering synthesizes TMQ in batch condensation polymerization reactor, TMQ receipts amount more normally feeds intake increase
0.5g；COD value of waste water is reduced to 14500mg/L after extraction, while the smell of waste water reduces；After pretreatment, Ke Yijin
Row desalting processing, to desalter without blocking；Extractant TMQ monomers are reaction intermediate, can directly be recycled, loss
Measure small, simple to operation, feature of environmental protection height.
The invention is not limited in above-mentioned embodiment, above-mentioned embodiment is only schematical,
It is not restricted, one of ordinary skill in the art is not departing from present inventive concept and right under the enlightenment of the present invention
It is required that under the ambit protected, the specific conversion of many forms can also be made, these belong to the protection model of the present invention
Within enclosing.
Claims (2)
1. a kind of method of material recycle in rubber antioxidant TMQ productions waste water, it is characterized in that by the waste water after neutralization by quiet
After putting layering, aqueous phase containing floccule adds extractant, stratification after extraction, and aqueous phase is uniformly processed into sewage disposal system,
Oil phase returns to reuse in batch condensation polymerization reactor；Described extractant with containing in floccule and the weight ratio of waste water is 1-20:1；Institute
The extractant stated is aniline, TMQ synthons or Synthesis liquid；Described extraction temperature is 30-95 DEG C；Described extraction time is
0.5-2h；The stratification time is 0.5-4h after described extraction.
2. the method as described in claim 1, it is characterized in that adding extractant to aqueous phase containing floccule under conditions of stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510964282.1A CN105502740B (en) | 2015-12-17 | 2015-12-17 | A kind of method of material recycle in rubber antioxidant TMQ productions waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510964282.1A CN105502740B (en) | 2015-12-17 | 2015-12-17 | A kind of method of material recycle in rubber antioxidant TMQ productions waste water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105502740A CN105502740A (en) | 2016-04-20 |
| CN105502740B true CN105502740B (en) | 2018-03-09 |
Family
ID=55711125
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510964282.1A Active CN105502740B (en) | 2015-12-17 | 2015-12-17 | A kind of method of material recycle in rubber antioxidant TMQ productions waste water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105502740B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240341A (en) * | 2019-06-25 | 2019-09-17 | 运城晋腾化学科技有限公司临猗分公司 | A kind of waste water treatment system and method for hydrochloric acid catalysis synthesis RD anti-aging agent |
| CN112661331A (en) * | 2019-10-15 | 2021-04-16 | 中石化南京化工研究院有限公司 | Method for recycling materials in anti-aging agent TMQ production wastewater |
| CN114259749B (en) * | 2022-02-28 | 2022-06-07 | 东营威联化学有限公司 | Online desalination device of fractionating tower top circulation system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997009276A1 (en) * | 1995-08-22 | 1997-03-13 | The Louisiana Land And Exploration Company | Waste treatment and minimization system |
| CN1436731A (en) * | 2003-03-25 | 2003-08-20 | 武汉化工学院 | Processing method of organic waste water containing high-concentration inorganic acid |
| CN101353213A (en) * | 2007-07-25 | 2009-01-28 | 中国石油天然气股份有限公司 | Method for treating octanol waste lye by miscellaneous alcohol acidization-extraction method |
| CN102161546A (en) * | 2010-12-31 | 2011-08-24 | 河南省华鼎高分子合成树脂有限公司 | Method for processing production effluent of maleimide compound |
| CN102936051A (en) * | 2012-11-19 | 2013-02-20 | 上海百菲特环保科技有限公司 | Process for treating dinaphthol wastewater by using complexation extraction method |
-
2015
- 2015-12-17 CN CN201510964282.1A patent/CN105502740B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997009276A1 (en) * | 1995-08-22 | 1997-03-13 | The Louisiana Land And Exploration Company | Waste treatment and minimization system |
| CN1436731A (en) * | 2003-03-25 | 2003-08-20 | 武汉化工学院 | Processing method of organic waste water containing high-concentration inorganic acid |
| CN101353213A (en) * | 2007-07-25 | 2009-01-28 | 中国石油天然气股份有限公司 | Method for treating octanol waste lye by miscellaneous alcohol acidization-extraction method |
| CN102161546A (en) * | 2010-12-31 | 2011-08-24 | 河南省华鼎高分子合成树脂有限公司 | Method for processing production effluent of maleimide compound |
| CN102936051A (en) * | 2012-11-19 | 2013-02-20 | 上海百菲特环保科技有限公司 | Process for treating dinaphthol wastewater by using complexation extraction method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105502740A (en) | 2016-04-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105502740B (en) | A kind of method of material recycle in rubber antioxidant TMQ productions waste water | |
| CN102092906B (en) | Treatment and resource-utilizing technology of tert-butyl peroxy benzoate production wastewater | |
| CN104724892A (en) | Treatment method of acidic dye industrial wastewater | |
| CN104193108B (en) | Produce the treatment process of washes in tetrabromo-bisphenol process | |
| Expósito et al. | Solar photo-degradation of a pharmaceutical wastewater effluent in a semi-industrial autonomous plant | |
| CN113185487B (en) | Production process of Jiale musk | |
| CN105036493A (en) | Sewage treatment method | |
| CN106349043A (en) | Attenuant acetaldehyde rectification residual liquor recycling method | |
| CN101012092A (en) | Process for treating furfural waste water | |
| CN107857444A (en) | A kind of environment protection method for handling dyeing waste water | |
| CN107020146A (en) | A kind of composite catalyst for handling phenolic waste water and preparation method thereof | |
| CN102092903A (en) | Process for treating and recycling di-tertiary-butyl peroxide production waste water | |
| CN109607915A (en) | A kind of processing method of Benzotriazole Ultraviolet Stabilizer production waste water | |
| CN108238647A (en) | The process units of coagulant polymeric ferric sulfate | |
| CN103893941B (en) | Utilize alkaline residue treatment of wastes with processes of wastes against one another neutralizing hydrolysis to process the method for organic silicon slurry slag | |
| CN103804264B (en) | The method processing DCP crystalline mother solution | |
| CN102092905A (en) | Process for treating and recycling industrial wastewater of peroxide-2-ethylhexoic acid tertiary butyl ester | |
| CN113402381A (en) | Preparation method of chloroacetyl chloride | |
| CN104528772A (en) | Innocent treatment method for producing solid wastes by using metformin hydrochloride | |
| JP2010131489A (en) | Method of treating aromatic amines-containing wastewater | |
| CN105417786B (en) | Processing method containing 2 chloroethyl propyl ether waste water | |
| CN104692594B (en) | A kind of recycled polyester produces the processing method of waste water | |
| CN205204954U (en) | Equipment of polymerization mother liquor preliminary treatment chlorination mother liquor | |
| CN216191569U (en) | Epoxy resin high salt waste water multi-stage treatment system | |
| CN216584626U (en) | Bio-based auxiliary agent waste water treatment system |
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 |