CN111362840A - Method for recycling ammonia from accelerator DPG mother liquor in production process to synthesize accelerator DPG through recycling - Google Patents
Method for recycling ammonia from accelerator DPG mother liquor in production process to synthesize accelerator DPG through recycling Download PDFInfo
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- CN111362840A CN111362840A CN202010292614.7A CN202010292614A CN111362840A CN 111362840 A CN111362840 A CN 111362840A CN 202010292614 A CN202010292614 A CN 202010292614A CN 111362840 A CN111362840 A CN 111362840A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
- C01C1/028—Preparation of ammonia from inorganic compounds from ammonium sulfate or sulfite
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Abstract
The invention provides a method for recycling ammonia from mother liquor for producing an accelerator DPG to recycle and synthesize the accelerator DPG, which is characterized in that the mother liquor obtained by producing the accelerator DPG is pumped into a distillation still from a mother liquor tank, excessive calcium oxide is added into the distillation still to be stirred and reacted for 4 to 6 hours, then the temperature is raised to 80 to 100 ℃, and the normal pressure distillation is carried out; and (3) recovering ammonia gas through an ammonia gas recovery device, and directly using the ammonia water for producing the accelerator DPG in the next flow after the mass concentration of the recovered ammonia water is more than 25%. The method recycles the mother liquor, improves the utilization rate of raw materials, can greatly reduce the discharge amount of the wastewater and improve the quality of the wastewater, can meet the requirements of European REACH regulations and national relevant protection policies while meeting the environmental protection requirements, effectively protects the body health of staff, and can reduce the pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for recycling ammonia from a mother liquor for producing an accelerator DPG to recycle and synthesize the accelerator DPG.
Background
The rubber vulcanization accelerator DPG is an important rubber medium-speed vulcanization accelerator with the chemical name of diphenylguanidine, and is mainly used as the vulcanization accelerator of natural rubber and synthetic rubber; it can also be used as activator of thiazole thiuram and sulfenamide accelerator. When used in combination with DM and TMTD, can be used for continuous vulcanization. The chloroprene rubber can also play the roles of a plasticizer and a peptizer, and is mainly used for manufacturing rubber products such as tires, rubber plate soles and the like. At present, domestic enterprises producing rubber vulcanization accelerator DPG generally use a production process of an oxygen oxidation method, the process can generate a large amount of waste water, the main components of the waste water are excessive ammonia water and a byproduct ammonium sulfate, and the treatment is complex and difficult; under the large environment with gradually improved environmental protection requirements, the production of the rubber vulcanization accelerator DPG is greatly limited, a long-term short supply and short demand state appears, and as a worldwide rubber processing industry in China, the rubber vulcanization accelerator DPG plays a very important role in rubber production, so that the development of the production process of the rubber vulcanization accelerator DPG towards green and environment-friendly development is an important research direction.
Disclosure of Invention
A method for recycling ammonia from mother liquor of accelerator DPG to recycle synthetic accelerator DPG so as to achieve the purposes of reducing the production cost of accelerator DPG, improving the utilization rate of raw materials and reducing the discharge of three wastes.
A method for recycling ammonia from mother liquor for producing an accelerator DPG to recycle and synthesize the accelerator DPG is characterized in that the mother liquor obtained by producing the accelerator DPG is pumped into a distillation kettle from a mother liquor tank, excessive calcium oxide is added into the distillation kettle, stirred and reacted for 4 to 6 hours, then the temperature is raised to 80 to 100 ℃, and the normal pressure distillation is carried out; ammonia gas is recovered through an ammonia gas recovery device, and after the mass concentration of the recovered ammonia water is more than 25%, the ammonia water is directly used for producing an accelerator DPG in the next process;
ammonia recovery unit be mother liquor tank tube coupling with the pump, the pump is connected to the stills, tube coupling to ammonia recovery unit in the stills: water is contained in the primary receiving tank, and a pipeline for connecting the distillation kettle to the primary receiving tank is extended to a position below the water level; a discharge pipeline is connected to the bottom of the primary receiving tank to supply ammonia water for the next production process; a pump is arranged in another circulating pipeline connected with the bottom of the primary receiving tank; the circulating pipeline is connected to the first-stage falling film absorber, a discharging pipeline is connected to the first-stage receiving tank at the bottom of the first-stage falling film absorber, a connecting pipeline is connected to the other ammonia gas absorption unit at the top of the first-stage falling film absorber and is connected to the position below the water level in the second-stage receiving tank, a discharging pipe is connected to the bottom of the second-stage receiving tank, a pump is mounted in the discharging pipe, the outlet pipe of the pump is divided into two parts, one discharging pipe is connected to the first-stage receiving tank, the other discharging pipeline is connected to the top end of the second-stage falling film absorber, the discharging pipe is connected to the second-stage receiving tank at the bottom of the second-stage falling film absorber, and the pipeline is connected to the next-stage ammonia gas absorption; the top end of the last stage falling film absorber is connected with an emptying pipeline, and a water replenishing pipeline is connected to the last stage receiving tank.
Preferably, the atmospheric distillation time is 3-4 h.
Preferably, the water supplemented in the water supplementing pipeline is primary water.
Preferably, the accelerator DPG is produced by the following steps:
step 1: mixing diphenylthiourea with water in a high-pressure kettle, then adding a mixed solution of copper acetate and ammonia water, introducing oxygen gas with the pressure of 0.1-0.6MPa, and raising the temperature when the pressure in the kettle reaches 0.8-0.9 MPa; reacting at 50-65 deg.C for 4-6 times of oxygen introduction for 4-8 hr to obtain the primary product of accelerator DPG;
wherein: the weight ratio of the diphenylthiourea to the water to the copper acetate to the ammonia water to the oxygen is (200-300): (200-400): (10-50): (50-100): (50-70); the concentration of ammonia water is 25%;
step 2: filtering the primary accelerator DPG product obtained in the step (1) to obtain a crude product, and collecting mother liquor into a mother liquor tank;
and step 3: dissolving the crude product with 10% dilute acid, filtering to remove insoluble impurities, dripping dilute alkali liquor into the filtrate to precipitate pure accelerator DPG, filtering, and washing to obtain qualified product, namely accelerator DPG;
wherein the concentration of the dilute hydrochloric acid is 10 percent, the molar ratio of the hydrochloric acid to the diphenylthiourea is 1:1, and the molar ratio of the addition amount of the dilute alkali solution to the hydrochloric acid is 1: 1.
Preferably, when the mixed solution of copper acetate and ammonia water is prepared, copper acetate is added into dissolved ammonia water to form the mixed solution.
Preferably, the mass ratio of the added calcium oxide to the generated ammonium sulfate is: 600: 110.
preferably, the ammonia gas absorption unit in the ammonia gas recovery device has three stages.
The invention has the beneficial effects that:
adding calcium oxide into mother liquor for producing the accelerator DPG, converting ammonium sulfate which is a byproduct in the production of the accelerator DPG into ammonia water and calcium sulfate precipitate, distilling the mother liquor to recover ammonia, wherein the yield of ammonia gas reaches 80%, when the concentration of the ammonia water reaches more than 25%, the ammonia water is used as a raw material for synthesizing the accelerator DPG again, and the residual calcium sulfate solid is treated as waste solid. The concentration of the prepared ammonia water after multiple recovery meets the production condition, and the ammonia water is continuously used for the synthesis of DPG. The method recycles the mother liquor, improves the utilization rate of raw materials, can greatly reduce the discharge amount of the wastewater and improve the quality of the wastewater, can meet the requirements of European REACH regulations and national relevant protection policies while meeting the environmental protection requirements, effectively protects the body health of staff, and can reduce the pollution to the environment.
Drawings
FIG. 1 is a schematic view of an ammonia gas recovery apparatus according to the present invention.
In the figure: 1. a mother liquor tank; 2. a distillation kettle; 3. a primary receiving tank; 4. a first-order falling film absorber; 5. a secondary receiving tank; 6. a secondary falling film absorber; 7. a third-stage receiving tank; 8. three-stage falling film absorber.
Detailed Description
Example 1
In the method for recycling ammonia from mother liquor in producing accelerator DPG to recycle synthetic accelerator DPG again, an ammonia recovery device is characterized in that a mother liquor tank 1 is connected with a pump through a pipeline, the pump is connected to a distillation still 2, and a pipeline in the distillation still 2 is connected to an ammonia recovery unit: water is contained in the primary receiving tank 3, and the distillation kettle 2 is connected into a pipeline of the primary receiving tank 3 and extends to a position below the water level; a discharge pipeline is connected to the bottom of the primary receiving tank 3 to supply ammonia water for the next production process; a pump is arranged in another circulating pipeline connected with the bottom of the first-stage receiving tank 3; a circulating pipeline is connected to the primary falling film absorber 4, a discharging pipeline is connected to the primary receiving tank 3 at the bottom of the primary falling film absorber 4, a connecting pipeline is connected to the other ammonia gas absorption unit at the top of the primary falling film absorber 4, the connecting pipeline is connected to the position below the water level in the secondary receiving tank 5 at the top of the primary falling film absorber 4, a discharging pipe is connected to the bottom of the secondary receiving tank 3, a pump is mounted in the discharging pipe, an outlet pipe of the pump is divided into two parts, one discharging pipe is connected to the primary receiving tank 3, the other discharging pipeline is connected to the top end of the secondary falling film absorber 6, the discharging pipe is connected to the secondary receiving tank 5 at the bottom of the secondary falling film absorber 6, and a pipeline is connected to the next ammonia gas absorption unit at the top end of the secondary falling film absorber 6; the top end of the second-stage falling film absorber 6 is connected with a pipeline below the water level in the third-stage receiving tank 7, a discharge pipe is connected to the bottom of the third-stage receiving tank 7, a pump is mounted in the discharge pipe, an outlet pipe of the pump is divided into two parts, one discharge pipe is connected to the second-stage receiving tank 5, the other discharge pipe is connected to the top end of the third-stage falling film absorber 8, and the discharge pipe is connected to the third-stage receiving tank 7 at the bottom of the third-stage falling film absorber 8; an emptying pipeline is connected to the top end of the three-stage falling film absorber 8, and a water replenishing pipeline is connected to the three-stage receiving tank 7 to replenish primary water.
Example 2
A method for recycling ammonia from mother liquor in producing accelerator DPG to recycle synthetic accelerator DPG comprises the following steps:
step 1: mixing diphenylthiourea with water in a high-pressure kettle, adding copper acetate into dissolved ammonia water to form a mixed solution, adding the mixed solution into the high-pressure kettle, introducing oxygen under the pressure of 0.1-0.6MPa, and raising the temperature until the pressure in the kettle reaches 0.8-0.9 MPa; reacting at 50-65 deg.C for 4-6 times of oxygen introduction for 4-8 hr to obtain the primary product of accelerator DPG;
wherein: the weight ratio of the diphenylthiourea to the water to the copper acetate to the ammonia water to the oxygen is (200-300): (200-400): (10-50): (50-100): (50-70); the concentration of ammonia water is 25%;
step 2: filtering the primary accelerator DPG product obtained in the step (1) to obtain a crude product, and collecting mother liquor into a mother liquor tank;
pumping the mother liquor into a distillation kettle, adding excessive calcium oxide into the distillation kettle, stirring and reacting for 4-6 hours, then heating to 80-100 ℃, and distilling for 3-4 hours under normal pressure; ammonia gas is recovered through an ammonia gas recovery device, the mass concentration of the recovered ammonia water is 26%, and the ammonia water is directly used for producing an accelerator DPG in the next process;
and step 3: dissolving the crude product with 10% diluted acid, filtering to remove insoluble impurities, dripping diluted alkaline solution into the filtrate to separate out pure DPG, filtering, and washing with water to obtain qualified product;
wherein the concentration of the dilute hydrochloric acid is 10 percent, the molar ratio of the hydrochloric acid to the diphenylthiourea is 1:1, and the molar ratio of the addition amount of the dilute alkali solution to the hydrochloric acid is 1: 1.
Example 3
The procedure of example 2 was followed except that copper acetate was added to the aqueous ammonia recovered in example 2 in step 1 to form a mixed solution, and the other production steps were carried out. And comparing the obtained accelerator DPG product with the accelerator DPG product obtained in example 2 on various detection values, see Table 1, no obvious difference exists, and the method is practical and feasible.
Table 1:
| the product yield is% | Purity% | Melting Point C | Ash content% | Percent of screen residue | |
| Example 2 group 1 | 92.0 | 98.5 | 145.5 | 0.20 | 0.07 |
| EXAMPLE 2 group 2 | 91.8 | 98.4 | 145.3 | 0.18 | 0.08 |
| Example 2 group 3 | 92.1 | 98.2 | 145.0 | 0.16 | 0.06 |
| Example 3 group 1 | 91.6 | 98.0 | 145.0 | 0.15 | 0.06 |
| EXAMPLE 3 group 2 | 92.0 | 98.3 | 145.4 | 0.17 | 0.08 |
| Example 3 group 3 | 92.2 | 98.5 | 145.5 | 0.20 | 0.07 |
Claims (7)
1. A method for recycling ammonia from mother liquor for producing an accelerator DPG to recycle and synthesize the accelerator DPG is characterized in that the mother liquor obtained by producing the accelerator DPG is pumped into a distillation kettle from a mother liquor tank, excessive calcium oxide is added into the distillation kettle, stirred and reacted for 4 to 6 hours, then the temperature is raised to 80 to 100 ℃, and the normal pressure distillation is carried out; ammonia gas is recovered through an ammonia gas recovery device, and after the mass concentration of the recovered ammonia water is more than 25%, the ammonia water is directly used for producing an accelerator DPG in the next process;
ammonia recovery unit be mother liquor tank tube coupling with the pump, the pump is connected to the stills, tube coupling to ammonia recovery unit in the stills: water is contained in the primary receiving tank, and a pipeline for connecting the distillation kettle to the primary receiving tank is extended to a position below the water level; a discharge pipeline is connected to the bottom of the primary receiving tank to supply ammonia water for the next production process; a pump is arranged in another circulating pipeline connected with the bottom of the primary receiving tank; the circulating pipeline is connected to the first-stage falling film absorber, a discharging pipeline is connected to the first-stage receiving tank at the bottom of the first-stage falling film absorber, a connecting pipeline is connected to the other ammonia gas absorption unit at the top of the first-stage falling film absorber and is connected to the position below the water level in the second-stage receiving tank, a discharging pipe is connected to the bottom of the second-stage receiving tank, a pump is mounted in the discharging pipe, the outlet pipe of the pump is divided into two parts, one discharging pipe is connected to the first-stage receiving tank, the other discharging pipeline is connected to the top end of the second-stage falling film absorber, the discharging pipe is connected to the second-stage receiving tank at the bottom of the second-stage falling film absorber, and the pipeline is connected to the next-stage ammonia gas absorption; the top end of the last stage falling film absorber is connected with an emptying pipeline, and a water replenishing pipeline is connected to the last stage receiving tank.
2. The method for recycling ammonia from mother liquor in producing accelerator DPG for recycling synthetic accelerator DPG according to claim 1, wherein the atmospheric distillation time is 3-4 h.
3. The method for recycling ammonia generated in the production of accelerator DPG as well as the synthesis accelerator DPG, as claimed in claim 1, wherein the water supplemented in the water supplementing pipeline is primary water.
4. The method for recycling ammonia for recycling synthesis accelerator DPG from mother liquor in accelerator DPG production as claimed in claim 1, wherein the accelerator DPG is produced by the following steps:
step 1: mixing diphenylthiourea with water in a high-pressure kettle, then adding a mixed solution of copper acetate and ammonia water, introducing oxygen gas with the pressure of 0.1-0.6MPa, and raising the temperature when the pressure in the kettle reaches 0.8-0.9 MPa; reacting at 50-65 deg.C for 4-6 times of oxygen introduction for 4-8 hr to obtain the primary product of accelerator DPG;
wherein: the weight ratio of the diphenylthiourea to the water to the copper acetate to the ammonia water to the oxygen is (200-300): (200-400): (10-50): (50-100): (50-70); the concentration of ammonia water is 25%;
step 2: filtering the primary accelerator DPG product obtained in the step (1) to obtain a crude product, and collecting mother liquor into a mother liquor tank;
and step 3: dissolving the crude product with 10% dilute acid, filtering to remove insoluble impurities, dripping dilute alkali liquor into the filtrate to precipitate pure accelerator DPG, filtering, and washing to obtain qualified product, namely accelerator DPG;
wherein the concentration of the dilute hydrochloric acid is 10 percent, the molar ratio of the hydrochloric acid to the diphenylthiourea is 1:1, and the molar ratio of the addition amount of the dilute alkali solution to the hydrochloric acid is 1: 1.
5. The method for producing the accelerator DPG mother liquor to recover ammonia and recycle the synthesis accelerator DPG as claimed in claim 4, wherein the copper acetate is added into the dissolved amount of ammonia water to form a mixed solution when the mixed solution of the copper acetate and the ammonia water is prepared.
6. The method for recycling ammonia generated in the production of accelerator DPG mother liquor for recycling synthetic accelerator DPG as claimed in claim 1, wherein the mass ratio of the added calcium oxide to the generated ammonium sulfate is as follows: 600: 110.
7. the method for recycling ammonia generated in the production of accelerator DPG as well as synthesizing accelerator DPG according to the claim 1, wherein the ammonia absorption unit in the ammonia recovery device is three-stage.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1657428A (en) * | 2005-01-28 | 2005-08-24 | 江苏江大环境工程有限责任公司 | New comprehensive utilization method of ADC foaming agent condensed mother liquor |
| CN102358727A (en) * | 2011-08-29 | 2012-02-22 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization promoter diphenylguanidine by mother liquor use |
| CN103922926A (en) * | 2014-04-17 | 2014-07-16 | 绍兴县远程树脂科技有限公司 | Process for purifying residual solid waste generated after alkali peeling wastewater treatment |
| CN104193751A (en) * | 2014-07-25 | 2014-12-10 | 沈美忠 | Method for treating mother liquid discharged in glycine production |
| CN204778859U (en) * | 2015-06-05 | 2015-11-18 | 江阴市江中设备制造有限公司 | System for including retrieving ammonia in ammonia mother liquor |
| CN205035304U (en) * | 2015-09-25 | 2016-02-17 | 鹤壁市恒力橡塑股份有限公司 | Reduce production system that rubber vulcanization accelerator DPG liquid ammonia consumed |
| CN205258042U (en) * | 2015-11-30 | 2016-05-25 | 上虞大新色彩化工有限公司 | Synthetic mother liquor ammonia backwater device |
| CN108586295A (en) * | 2018-05-23 | 2018-09-28 | 科迈化工股份有限公司 | A kind of continuous production method of accelerator D PG |
-
2020
- 2020-04-15 CN CN202010292614.7A patent/CN111362840A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657428A (en) * | 2005-01-28 | 2005-08-24 | 江苏江大环境工程有限责任公司 | New comprehensive utilization method of ADC foaming agent condensed mother liquor |
| CN102358727A (en) * | 2011-08-29 | 2012-02-22 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization promoter diphenylguanidine by mother liquor use |
| CN103922926A (en) * | 2014-04-17 | 2014-07-16 | 绍兴县远程树脂科技有限公司 | Process for purifying residual solid waste generated after alkali peeling wastewater treatment |
| CN104193751A (en) * | 2014-07-25 | 2014-12-10 | 沈美忠 | Method for treating mother liquid discharged in glycine production |
| CN204778859U (en) * | 2015-06-05 | 2015-11-18 | 江阴市江中设备制造有限公司 | System for including retrieving ammonia in ammonia mother liquor |
| CN205035304U (en) * | 2015-09-25 | 2016-02-17 | 鹤壁市恒力橡塑股份有限公司 | Reduce production system that rubber vulcanization accelerator DPG liquid ammonia consumed |
| CN205258042U (en) * | 2015-11-30 | 2016-05-25 | 上虞大新色彩化工有限公司 | Synthetic mother liquor ammonia backwater device |
| CN108586295A (en) * | 2018-05-23 | 2018-09-28 | 科迈化工股份有限公司 | A kind of continuous production method of accelerator D PG |
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