CN114478335A - Method for recycling peptizer DBD from peptizer DBD waste - Google Patents
Method for recycling peptizer DBD from peptizer DBD waste Download PDFInfo
- Publication number
- CN114478335A CN114478335A CN202210119785.9A CN202210119785A CN114478335A CN 114478335 A CN114478335 A CN 114478335A CN 202210119785 A CN202210119785 A CN 202210119785A CN 114478335 A CN114478335 A CN 114478335A
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- CN
- China
- Prior art keywords
- peptizer
- dbd
- waste
- peptizer dbd
- toluene
- 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.)
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- 239000002699 waste material Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000007787 solid Substances 0.000 claims abstract description 49
- 239000000126 substance Substances 0.000 claims abstract description 38
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 229960001701 chloroform Drugs 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 239000012535 impurity Substances 0.000 abstract description 10
- 238000000935 solvent evaporation Methods 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 7
- 150000003839 salts Chemical class 0.000 abstract description 6
- ZHMIOPLMFZVSHY-UHFFFAOYSA-N n-[2-[(2-benzamidophenyl)disulfanyl]phenyl]benzamide Chemical compound C=1C=CC=CC=1C(=O)NC1=CC=CC=C1SSC1=CC=CC=C1NC(=O)C1=CC=CC=C1 ZHMIOPLMFZVSHY-UHFFFAOYSA-N 0.000 description 87
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000000967 suction filtration Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 description 1
- RALRVIPTUXSBPO-UHFFFAOYSA-N 4-[4-chloro-3-(trifluoromethyl)phenyl]piperidin-4-ol Chemical compound C=1C=C(Cl)C(C(F)(F)F)=CC=1C1(O)CCNCC1 RALRVIPTUXSBPO-UHFFFAOYSA-N 0.000 description 1
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- SRRKNRDXURUMPP-UHFFFAOYSA-N sodium disulfide Chemical compound [Na+].[Na+].[S-][S-] SRRKNRDXURUMPP-UHFFFAOYSA-N 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a method for recovering peptizer DBD from peptizer DBD waste, which comprises the following steps: mixing and dissolving DBD waste serving as a peptizer and trichloromethane, and then filtering to obtain a solution; evaporating the solvent from the solution to obtain a solid substance; and mixing the solid substance with toluene, and filtering to obtain the peptizer DBD. Dissolving organic matters and a peptizer DBD in peptizer waste by using trichloromethane, and filtering to remove inorganic salts and other insoluble impurities in the peptizer waste; most of raw materials and byproducts for preparing the peptizer DBD can be removed through solvent evaporation, and a solid substance containing a large amount of peptizer DBD is obtained; and finally, washing the solid substance by using toluene, and extracting other organic impurities to obtain the peptizer DBD solid, thereby achieving the purpose of recovering the peptizer DBD from the peptizer DBD waste.
Description
Technical Field
The invention belongs to the technical field of peptizer synthesis, and particularly relates to a method for recovering peptizer DBD from peptizer DBD waste.
Background
The peptizer DBD (2, 2' -dibenzamido diphenyl disulfide) is generally applied to rubber, can reduce the molecular weight of the rubber, shorten the plastication time, reduce the energy consumption and improve the production efficiency.
At present, the synthesis methods of peptizers DBD can be divided into two major categories: one is by hydrolysis of benzothiazole; the other type is that ortho-nitrochlorobenzene is used as a raw material, and a target product is prepared by reacting with sodium hydrosulfide, sodium disulfide, ammonium hydrosulfide, sodium disulfate and the like, wherein the total yield of the peptizer DBD in the two synthesis methods is only 85-90%, about 5-10% of the peptizer DBD enters a subsequent distillation system along with a solvent in washing and centrifuging processes for solvent recycling, and finally 5-10% of the peptizer DBD enters waste and cannot be recycled, so that the residue quantity is large, and the production cost is remarkably improved. Therefore, how to recover the peptizer DBD from the peptizer DBD waste becomes a difficult problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a method for recovering a peptizer DBD from peptizer DBD waste. The method provided by the invention can realize the recovery of the peptizer DBD from the peptizer DBD waste, and has high purity.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for recovering peptizer DBD from peptizer DBD waste, which comprises the following steps:
(1) mixing and dissolving DBD waste serving as a peptizer and trichloromethane, and then filtering to obtain a solution;
(2) evaporating the solvent of the solution obtained in the step (1) to obtain a solid substance;
(3) and (3) mixing the solid substance obtained in the step (2) with toluene, and then filtering to obtain the peptizer DBD.
Preferably, the mixing of the peptizer DBD waste and the chloroform in the step (1) is performed under stirring conditions.
Preferably, the stirring time is 0.5-2 h.
Preferably, the stirring time is 0.5-1 h.
Preferably, the temperature for solvent evaporation in the step (2) is 80-90 ℃.
Preferably, the temperature for evaporating the solvent is 80-85 ℃.
Preferably, the mass of the toluene in the step (3) is 10-20% of the mass of the solid substance.
Preferably, the mass of the toluene in the step (3) is 10-15% of the mass of the solid substance.
Preferably, the step (3) further comprises drying after the filtration is completed.
Preferably, the drying temperature is 80-100 ℃.
The invention provides a method for recovering peptizer DBD from peptizer DBD waste, which comprises the following steps: mixing and dissolving DBD waste serving as a peptizer and trichloromethane, and then filtering to obtain a solution; evaporating the solvent from the solution to obtain a solid substance; and mixing the solid substance with toluene, and filtering to obtain the peptizer DBD. Dissolving organic matters and a peptizer DBD in peptizer waste by using trichloromethane, and filtering to remove inorganic salts and other insoluble impurities in the peptizer waste; most of raw materials and byproducts for preparing the peptizer DBD can be removed through solvent evaporation, and a solid substance containing a large amount of peptizer DBD is obtained; and finally, washing the solid substance by using toluene, and extracting other organic impurities to obtain the peptizer DBD solid, thereby achieving the purpose of recovering the peptizer DBD from the peptizer DBD waste. Experimental results show that the melting point of the peptizer DBD recovered by the method provided by the invention is 141.7-142.8 ℃, the purity is more than 95%, the peptizer DBD can meet industrial standards, and the peptizer DBD meets the use requirements.
Detailed Description
The invention provides a method for recovering peptizer DBD from peptizer DBD waste, which comprises the following steps:
(1) mixing and dissolving DBD waste serving as a peptizer and trichloromethane, and then filtering to obtain a solution;
(2) evaporating the solvent of the solution obtained in the step (1) to obtain a solid substance;
(3) and (3) mixing the solid substance obtained in the step (2) with toluene, and then filtering to obtain the peptizer DBD.
The method provided by the invention is suitable for peptizer DBD waste generated by peptizer DBD prepared by any method. In the present invention, the peptizer DBD waste preferably includes raw materials, byproducts, inorganic salts and insoluble substances for producing the peptizer DBD.
According to the invention, the peptizer DBD waste is mixed with the trichloromethane for dissolving, and then the solution is obtained by filtering. The invention adopts trichloromethane to dissolve organic matters in the peptizer waste, including the peptizer DBD, and removes inorganic salts and other insoluble impurities in the peptizer DBD waste through filtration.
The source of the chloroform in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used. The dosage of the trichloromethane is not specially limited until the solid in the peptizer DBD waste is not dissolved any more.
In the present invention, the mixing of the peptizer DBD waste and the chloroform is preferably performed under stirring conditions; the stirring time is preferably 0.5-2 h, and more preferably 0.5-1 h; the stirring temperature is preferably 20-50 ℃. In the present invention, the stirring rate is not particularly limited, and may be determined based on common knowledge. According to the invention, the mixing of the peptizer DBD waste and the trichloromethane can dissolve organic matters in the peptizer waste.
The operation of the filtration is not particularly limited in the present invention, and a filtration operation known to those skilled in the art may be employed. According to the invention, inorganic salts and other insoluble impurities in the peptizer DBD waste can be removed through filtration. In the invention, the solution obtained by filtering comprises organic matters such as trichloromethane, a peptizer DBD, raw materials for preparing the peptizer DBD, byproducts and the like.
After obtaining the solution, the invention evaporates the solvent of the solution to obtain the solid substance. The invention adopts solvent evaporation to remove most of chloroform, raw materials for preparing the peptizer DBD, byproducts and other organic matters.
In the invention, the temperature for evaporating the solvent is preferably 80-90 ℃, and more preferably 80-85 ℃. In the present invention, the time for evaporating the solvent is not particularly limited, and the solvent may be evaporated until no fraction is separated. The invention can further improve the removal rate of other organic impurities and improve the purity of the peptizer DBD by controlling the temperature of solvent evaporation.
After the solid substance is obtained, the invention mixes the solid substance with toluene and filters to obtain the peptizer DBD. The invention adopts toluene to wash solid substances, and extracts other organic substances to obtain the peptizer DBD solid.
In the invention, the mass of the toluene is preferably 10-20% of the mass of the solid substance, and more preferably 10-15%. The toluene is not particularly limited in its source in the present invention, and commercially available products known to those skilled in the art may be used. The operation of mixing the solid substance and the toluene is not particularly limited, and the solid substance and the toluene can be uniformly mixed as long as the quality of the toluene meets the requirements. The operation of the filtration is not particularly limited in the present invention, and a filtration operation known to those skilled in the art may be employed.
After the filtration is finished, the invention preferably dries the solid obtained by the filtration to obtain the peptizer DBD.
In the invention, the drying temperature is preferably 80-100 ℃. The drying time is not specially limited, and the drying is carried out until the weight is constant.
In the present invention, the solid matter is mixed with toluene, and filtration preferably also gives a filtrate. In the present invention, the filtrate is preferably subjected to solvent evaporation to obtain a solid. In the present invention, the temperature for evaporating the solvent is preferably 90 to 110 ℃. In the present invention, the time for evaporating the solvent is not particularly limited, and the solvent may be evaporated until no fraction is separated. The invention can remove toluene in the filtrate by controlling solvent evaporation, thereby obtaining solid containing raw materials and byproducts, and the solid can be used for subsequent utilization according to composition.
Dissolving organic matters and a peptizer DBD in peptizer waste by using trichloromethane, and filtering to remove inorganic salts and other insoluble impurities in the peptizer waste; most of raw materials and byproducts for preparing the peptizer DBD can be removed through solvent evaporation, and a solid substance containing a large amount of the peptizer DBD is obtained; and finally, washing the solid substance by using toluene, and extracting other organic impurities to obtain the peptizer DBD solid, thereby achieving the purpose of recovering the peptizer DBD from the peptizer DBD waste.
According to the invention, the solvent is selected, chloroform is used for dissolving all organic matters in the waste, inorganic salt or insoluble impurities are filtered, toluene is used for washing, and the peptizer DBD is extracted completely, so that the peptizer DBD index is qualified.
The method provided by the invention is completely finished by using the solvent, so that the cost can be effectively saved, the heat required by solvent evaporation and recovery is little, and the waste is avoided; the chloroform has high solubility to organic matters, can be completely dissolved, ensures the recovery rate, is safe when used as an organic solvent, and is not like other solvents, flammable and explosive; toluene has a strong ability to dissolve organic substances other than the peptizer DBD and a low solubility to the peptizer DBD, and thus can be used as a detergent.
The method provided by the invention can reduce the production cost, recover materials, utilize subsequent tail waste, realize an environment-friendly process and solve the problems of high production cost and high content of the tail waste.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the 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.
Example 1
The method for recovering the peptizer DBD from the peptizer DBD waste comprises the following steps:
(1) adding 100g of peptizer DBD waste into a 1000mL beaker, adding 500mL of chloroform, stirring, and carrying out suction filtration to obtain a solution; wherein the stirring time is 60min, and the temperature is 20 ℃;
(2) evaporating the solvent of the solution obtained in the step (1) until no fraction appears to obtain a solid substance; wherein the solvent is evaporated at a temperature of 80 ℃;
(3) mixing 100mL of toluene with solid substances twice, washing, performing suction filtration, and drying to obtain a peptizer DBD; wherein the drying temperature is 80 ℃; the mass of toluene was 10% of the mass of the solid matter.
Example 2
The method for recovering the peptizer DBD from the peptizer DBD waste comprises the following steps:
(1) adding 100g of peptizer DBD waste into a 1000mL beaker, adding 1000mL of chloroform, stirring, and carrying out suction filtration to obtain a solution; wherein the stirring time is 60min, and the temperature is 20 ℃;
(2) evaporating the solvent of the solution obtained in the step (1) until no fraction appears to obtain a solid substance; wherein the solvent is evaporated at a temperature of 80 ℃;
(3) mixing 200mL of toluene with solid substances twice, washing, performing suction filtration, and drying to obtain a peptizer DBD; wherein the drying temperature is 80 ℃; the mass of toluene was 10% of the mass of the solid matter.
Example 3
The method for recovering the peptizer DBD from the peptizer DBD waste comprises the following steps:
(1) adding 500g of peptizer DBD waste into a 1000mL beaker, adding 2500mL of trichloromethane, stirring, and carrying out suction filtration to obtain a solution; wherein the stirring time is 60min, and the temperature is 20 ℃;
(2) evaporating the solvent of the solution obtained in the step (1) until no fraction appears to obtain a solid substance; wherein the solvent is evaporated at a temperature of 80 ℃;
(3) mixing 500mL of toluene with solid substances twice, washing, filtering, and drying to obtain a peptizer DBD; wherein the drying temperature is 80 ℃; the mass of toluene was 10% of the mass of the solid matter.
Example 4
The method for recovering the peptizer DBD from the peptizer DBD waste comprises the following steps:
(1) adding 500g of peptizer DBD waste into a 1000mL beaker, adding 3000mL of chloroform, stirring, and carrying out suction filtration to obtain a solution; wherein the stirring time is 60min, and the temperature is 20 ℃;
(2) evaporating the solvent of the solution obtained in the step (1) until no fraction appears to obtain a solid substance; wherein the solvent is evaporated at a temperature of 80 ℃;
(3) mixing 400mL of toluene with solid substances twice, washing, performing suction filtration, and drying to obtain a peptizer DBD; wherein the drying temperature is 80 ℃; the mass of toluene was 10% of the mass of the solid matter.
The performance data of the peptizers DBD prepared in examples 1-4 are shown in Table 1.
TABLE 1 Performance data of peptizers DBD prepared in examples 1-4
| Examples | Peptizer DBD weight (g) | Melting Point (industry Standard melting Point > 138 ℃ C.) | Purity of |
| 1 | 33 | Qualified, and the melting point is 142.5 DEG C | 98 |
| 2 | 30 | Qualified, the melting point is 142.8 DEG C | 98.5 |
| 3 | 35 | Qualified, and the melting point is 142 DEG C | 98.4 |
| 4 | 36 | Qualified, with a melting point of 141.7 DEG C | 98.2 |
The embodiment shows that the method provided by the invention can realize the recovery of the peptizer DBD, and the peptizer DBD obtained by recovery can meet the industrial standard and meet the use requirement.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for recovering peptizer DBD from peptizer DBD waste comprises the following steps:
(1) mixing and dissolving DBD waste serving as a peptizer and trichloromethane, and then filtering to obtain a solution;
(2) evaporating the solvent of the solution obtained in the step (1) to obtain a solid substance;
(3) and (3) mixing the solid substance obtained in the step (2) with toluene, and then filtering to obtain the peptizer DBD.
2. The method according to claim 1, wherein the mixing of the peptizer DBD waste and the chloroform in the step (1) is performed under stirring conditions.
3. The method according to claim 2, wherein the stirring time is 0.5-2 h.
4. The method according to claim 3, wherein the stirring time is 0.5-1 h.
5. The method according to claim 1, wherein the solvent is evaporated in the step (2) at a temperature of 80 to 90 ℃.
6. The method according to claim 5, wherein the solvent is evaporated at a temperature of 80-85 ℃.
7. The method according to claim 1, wherein the mass of the toluene in the step (3) is 10-20% of the mass of the solid substance.
8. The method according to claim 7, wherein the mass of the toluene in the step (3) is 10-15% of the mass of the solid substance.
9. The method of claim 1, wherein the step (3) further comprises drying after the filtering is completed.
10. The method according to claim 9, wherein the drying temperature is 80 to 100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210119785.9A CN114478335A (en) | 2022-02-09 | 2022-02-09 | Method for recycling peptizer DBD from peptizer DBD waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210119785.9A CN114478335A (en) | 2022-02-09 | 2022-02-09 | Method for recycling peptizer DBD from peptizer DBD waste |
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| Publication Number | Publication Date |
|---|---|
| CN114478335A true CN114478335A (en) | 2022-05-13 |
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|---|---|---|---|
| CN202210119785.9A Pending CN114478335A (en) | 2022-02-09 | 2022-02-09 | Method for recycling peptizer DBD from peptizer DBD waste |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106810480A (en) * | 2015-12-01 | 2017-06-09 | 青岛森美克化工技术有限公司 | A kind of green industrialized preparation method of rubber peptizer DBD |
| CN107868027A (en) * | 2016-09-26 | 2018-04-03 | 青岛九洲千和机械有限公司 | A kind of rubber peptizer DBD green industrialized preparation method |
| CN110511332A (en) * | 2019-07-30 | 2019-11-29 | 安徽华铂再生资源科技有限公司 | A kind of recovery process of discarded ABS plastic |
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2022
- 2022-02-09 CN CN202210119785.9A patent/CN114478335A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106810480A (en) * | 2015-12-01 | 2017-06-09 | 青岛森美克化工技术有限公司 | A kind of green industrialized preparation method of rubber peptizer DBD |
| CN107868027A (en) * | 2016-09-26 | 2018-04-03 | 青岛九洲千和机械有限公司 | A kind of rubber peptizer DBD green industrialized preparation method |
| CN110511332A (en) * | 2019-07-30 | 2019-11-29 | 安徽华铂再生资源科技有限公司 | A kind of recovery process of discarded ABS plastic |
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