CN107973385B - Environment-friendly flocculating agent and preparation method thereof - Google Patents
Environment-friendly flocculating agent and preparation method thereof Download PDFInfo
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- CN107973385B CN107973385B CN201711202886.8A CN201711202886A CN107973385B CN 107973385 B CN107973385 B CN 107973385B CN 201711202886 A CN201711202886 A CN 201711202886A CN 107973385 B CN107973385 B CN 107973385B
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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Abstract
The environment-friendly flocculant is applied to the production process of synthetic rubber as a substitute of CA, and is prepared from the following raw materials in parts by weight: 520-540 parts of epoxy chloropropane, 590-610 parts of a dimethylamine aqueous solution with the concentration of 40%, 500-520 parts of pure water, 22-26 parts of water-soluble chitosan with the deacetylation degree of 60%, 23-27 parts of isopropanol and 1.8-2.2 parts of a phosphorous acid catalyst, wherein the flocculant belongs to an environment-friendly high-molecular-weight flocculant, is free of formaldehyde components, reduces environmental pollution and harm to a human body, can reduce the COD (chemical oxygen demand) content of wastewater by 20-30%, and has the advantages of good energy saving and emission reduction effects, good flocculation effect, high coagulation speed and small dosage.
Description
Technical Field
The invention provides an environment-friendly flocculant and a preparation method thereof.
Background
In the prior production process of synthetic rubber, CA (dinitrile diamine formaldehyde condensate) is used as a flocculating agent, but the CA can generate formaldehyde in the process of coagulation to pollute the environment and harm human bodies, the total nitrogen content of the production wastewater using the CA flocculating agent is high and is difficult to degrade, and the total nitrogen content is 30m3The COD (chemical oxygen demand) content in/h reaches 800ppm, and CA has certain corrosivity to the equipment pipeline, needs to frequently check and maintain the running state of the equipment and timely handle the phenomenon of equipment running, falling, leaking and leaking caused by pipeline corrosion, and the workload of equipment maintenance is heavy. At present, flocculants containing formaldehyde are gradually banned from use.
Chitosan is obtained by deacetylation of chitin widely existing in the nature, and since 1859, after the first chitosan was obtained by Rouget of the french, the natural polymer is safe and environment-friendly, and its excellent properties such as biological functionality and compatibility, blood compatibility, safety, microbial degradability, etc. are widely concerned by various industries, and the application research in various fields such as medicine, food, chemical industry, cosmetics, water treatment, metal extraction and recovery, biochemistry and biomedical engineering, etc. has made a great progress. However, chitosan is expensive, has little influence on the performance of the synthetic rubber, is not convenient to be directly used in the coagulation process of the synthetic rubber, and has use value after being modified and used together with other chemicals; the research and development of the environment-friendly flocculating agent are also the key points of the research on the synthetic rubber auxiliary agent.
Disclosure of Invention
The invention aims to provide an environment-friendly flocculant and a preparation method thereof, wherein the flocculant can be used as a substitute of CA in the production process of synthetic rubber, so that the environmental pollution and the harm to human bodies are reduced, the energy-saving and emission-reducing effects are good, and the workload of maintenance is reduced.
The technical scheme of the invention is as follows: the environment-friendly flocculant is characterized by being prepared from the following raw materials in parts by weight: 520-540 parts of epoxy chloropropane, 590-610 parts of dimethylamine aqueous solution with the concentration of 40%, 500-520 parts of pure water, 22-26 parts of water-soluble chitosan with the deacetylation degree of 60%, 23-27 parts of isopropanol and 1.8-2.2 parts of phosphorous acid catalyst.
The environment-friendly flocculant is characterized by being prepared from the following raw materials in parts by weight: 530 parts of epichlorohydrin, 600 parts of dimethylamine aqueous solution with the concentration of 40%, 510 parts of pure water, 24 parts of water-soluble chitosan with the deacetylation degree of 60%, 25 parts of isopropanol and 2 parts of phosphorous acid catalyst.
The method for preparing the environment-friendly flocculant is characterized by comprising the following steps of:
1) adding 360 parts of pure water and a dimethylamine aqueous solution with the concentration of 40 percent into an enamel reaction kettle, adding isopropanol and a phosphorous acid catalyst, and controlling the internal vacuum degree of the reaction kettle to be 0.04 MPa-0.06 MPa;
2) preparing a metering tank A and a metering tank B, sucking epoxy chloropropane into the metering tank A in vacuum for standby, and sucking the dimethylamine aqueous solution with the residual concentration of 40% into the metering tank B in vacuum for standby;
3) starting an enamel reaction kettle to stir continuously under normal temperature environment, dropwise adding 45-50 parts per hour, dropwise adding epoxy chloropropane into the enamel reaction kettle through a metering tank A, dropwise adding 25-35 parts per hour, dropwise adding a dimethylamine aqueous solution with the concentration of 40% into the reaction kettle through a metering tank B, controlling the temperature in the reaction kettle to be 46-50 ℃ by using circulating water until the epoxy chloropropane and the dimethylamine aqueous solution with the concentration of 40% are completely dropwise added, adding water-soluble chitosan with the deacetylation degree of 60% into the reaction kettle, continuously stirring for 2 hours, stopping reaction, and obtaining a flocculant finished product.
The invention uses the polyepoxy-amine copolymer as the main component of the environment-friendly flocculant. Epichlorohydrin and dimethylamine are polymerized to form the framework of the environment-friendly flocculant. A small amount of water-soluble chitosan with deacetylation degree of 60 percent is used as polyamine and reacts with excessive epichlorohydrin to form modified chitosan, and the cation center density of the flocculant can be adjusted; meanwhile, the water-soluble chitosan has certain coagulation capacity and can be used as an auxiliary flocculant. Both the isopropanol and phosphorous acid catalysts function to compatibilize the monomers and catalyze the reaction. Isopropanol also has the effect of adjusting the viscosity of the product. After the water-soluble chitosan is added, the polymerization reaction of the epichlorohydrin and the dimethylamine is better controlled, the requirements on the charging proportion and the temperature control are greatly reduced, and the investment and the labor cost of a reaction device are saved.
The environment-friendly flocculant of the invention also has the advantages that: the environment-friendly flocculant (EEDC) belongs to an environment-friendly high-molecular-weight flocculant, has no formaldehyde component, reduces environmental pollution and harm to human bodies, can reduce the COD content of wastewater by 20-30%, has good energy-saving and emission-reducing effects, and can form more cation centers than the traditional CA flocculant due to the high molecular weight and good stability of the polyepoxy-amine copolymer and the matching of the water-soluble chitosan with the deacetylation degree of 60%, so that the flocculation effect is better, the coagulation speed is high, and the using amount is less. Compared with the dosage of CA, the dosage of the flocculant can be reduced by 30-40%, the preparation frequency is reduced, the labor intensity is reduced, the corrosion of the polyepoxy-amine copolymer to equipment pipelines is low, and the workload of maintenance is reduced, so that the environment-friendly flocculant disclosed by the invention is applied to the production of synthetic rubber, has low pollution and low corrosion, can save resources, and reduces wastes and environmental harmful substances.
The environment-friendly flocculant (EEDC) prepared according to the weight part ratio of the raw materials can stably reach the following technical indexes:
| specification items | Index (I) |
| Appearance of the product | Colorless or pale yellow transparent liquid |
| Solid content% | 50±2 |
| Viscosity (25 ℃ C.) mm2/S | 10-50 |
| pH value (1% aqueous solution) | 7-9 |
| Dimethylamine and epichlorohydrin condensate% | ≥35 |
In the preparation method of the invention, the purposes and advantages of controlling the vacuum degree in the kettle and limiting the vacuum degree value are as follows: through controlling vacuum in the reation kettle, having reduceed the oxygen content in the reation kettle, inject vacuum value and enable the dimethylamine raw materials of low boiling point and do not take place the flash explosion, guarantee the safety in production, simultaneously can be convenient inhale the material in the reation kettle.
In the preparation method, 40 percent dimethylamine aqueous solution and water are partially mixed, and then the other materials are dripped, so that the preparation method has the following purposes and advantages: partial raw materials in the reaction kettle are premixed in advance, and the rest raw materials are added, so that the dimethylamine raw material is slightly excessive, the side reaction is reduced, the initial viscosity of the reaction system can be reduced, and the phenomena of implosion reaction and temperature runaway are prevented.
In the preparation method of the invention, the purpose and the advantage of dropwise adding reactants are as follows: the reaction raw materials are added in a continuous dropwise adding and feeding mode, so that the feeding amount can be accurately measured, the accuracy of the reaction feeding ratio is ensured, the reaction temperature and heat release can be stably controlled, the occurrence of side reactions is reduced, the product yield is improved, the effective components of the product are increased, and the product quality is ensured. And the continuous feeding speed can be controlled according to the production load and the environmental temperature, so that the smooth reaction and the production efficiency are ensured. The purpose of adding the isopropanol is to adjust the viscosity of the EEDC product, control the vulcanization speed of rubber and the size of a rubber chain in the process of producing synthetic rubber, prevent the rubber from forming too fast and preventing overlarge rubber lumps from blocking a pipeline to influence production, and ensure that the production is carried out smoothly. The phosphorous acid catalyst can ensure that the reaction is carried out stably, can control the reaction speed in the reaction, prevent the bumping phenomenon generated by the over-fast reaction and avoid the accidents caused by the difficulty in controlling the over-high temperature. The low molecular weight water-soluble chitosan is adopted, so that the chitosan can enter a reaction system to be modified. The chitosan with the deacetylation degree of 60% is adopted, so that enough active amino groups can be ensured to participate in the reaction, and a cation center can be formed.
Method for using environment-friendly flocculating agent
The use method of the flocculant comprises the following steps: according to the addition of 3 kg per ton, the stock solution (solution with the content of 50%) is firstly prepared into 5% aqueous solution, 180L of the stock solution per hour is added into the coagulating bottom liquid, the synthetic rubber can be condensed out by matching with dilute acid, and the synthetic rubber is washed and dried to produce qualified products.
Detailed Description
The first embodiment is as follows:
1) 520 kg of epoxy chloropropane, 590 kg of dimethylamine aqueous solution with the concentration of 40 percent, 500 kg of pure water, 22 kg of water-soluble chitosan with the deacetylation degree of 60 percent, 23 kg of isopropanol and 1.8 kg of phosphorous acid catalyst are prepared as raw materials.
2) Adding 360 kilograms of pure water and a dimethylamine aqueous solution with the concentration of 40 percent into an enamel reaction kettle, adding isopropanol and a phosphorous acid catalyst, and controlling the internal vacuum degree of the reaction kettle to be 0.04 MPa;
3) preparing a metering tank A and a metering tank B, sucking epoxy chloropropane into the metering tank A in vacuum for standby, and sucking the dimethylamine aqueous solution with the residual concentration of 40% into the metering tank B in vacuum for standby;
4) under the normal temperature environment, starting an enamel reaction kettle for continuous stirring, dropwise adding 45 kilograms of epoxy chloropropane per hour, dropwise adding 25 kilograms of epoxy chloropropane per hour into the enamel reaction kettle through a metering tank A, dropwise adding a dimethylamine aqueous solution with the concentration of 40% into the enamel reaction kettle through a metering tank B, controlling the temperature in the enamel reaction kettle by using circulating water at 46 ℃ until the epoxy chloropropane and the dimethylamine aqueous solution with the concentration of 40% are completely dropwise added, adding water-soluble chitosan with the deacetylation degree of 60% into the enamel reaction kettle, continuously stirring for 2 hours, and stopping the reaction to obtain the flocculant finished product.
The second embodiment is as follows:
1) 530 kg of epoxy chloropropane, 600 kg of dimethylamine aqueous solution with the concentration of 40 percent, 510 kg of pure water, 24 kg of water-soluble chitosan with the deacetylation degree of 60 percent, 25 kg of isopropanol and 2 kg of phosphorous acid catalyst are prepared.
2) Adding 360 kilograms of pure water and a dimethylamine aqueous solution with the concentration of 40 percent into an enamel reaction kettle, adding isopropanol and a phosphorous acid catalyst, and controlling the internal vacuum degree of the reaction kettle to be 0.05 MPa;
3) preparing a metering tank A and a metering tank B, sucking epoxy chloropropane into the metering tank A in vacuum for standby, and sucking the dimethylamine aqueous solution with the residual concentration of 40% into the metering tank B in vacuum for standby;
4) starting an enamel reaction kettle to stir continuously under normal temperature environment, dripping 48 kilograms of epoxy chloropropane into the enamel reaction kettle per hour through a metering tank A, dripping 30 kilograms of epoxy chloropropane into the enamel reaction kettle per hour through a metering tank B, dripping 40 percent dimethylamine aqueous solution into the enamel reaction kettle through a metering tank B, controlling the temperature in the enamel reaction kettle to be 48 ℃ by using circulating water in the process until the epoxy chloropropane and the 40 percent dimethylamine aqueous solution are completely dripped, adding water-soluble chitosan with the deacetylation degree of 60 percent into the enamel reaction kettle, continuously stirring for 2 hours, and stopping reaction to obtain the flocculant finished product.
The third concrete embodiment:
1) 540 kg of epoxy chloropropane, 610 kg of a dimethylamine aqueous solution with the concentration of 40 percent, 520 kg of pure water, 26 kg of water-soluble chitosan with the deacetylation degree of 60 percent, 27 kg of isopropanol and 2.2 kg of a phosphorous acid catalyst are prepared as raw materials.
2) Adding 360 kilograms of pure water and a dimethylamine aqueous solution with the concentration of 40 percent into an enamel reaction kettle, adding isopropanol and a phosphorous acid catalyst, and controlling the internal vacuum degree of the reaction kettle to be 0.06 MPa;
3) preparing a metering tank A and a metering tank B, sucking epoxy chloropropane into the metering tank A in vacuum for standby, and sucking the dimethylamine aqueous solution with the residual concentration of 40% into the metering tank B in vacuum for standby;
4) under the normal temperature environment, starting an enamel reaction kettle for continuous stirring, dropwise adding 50 kilograms of epoxy chloropropane per hour, dropwise adding 35 kilograms of epoxy chloropropane per hour into the enamel reaction kettle through a metering tank A, dropwise adding 40 percent dimethylamine aqueous solution into the enamel reaction kettle through a metering tank B, controlling the temperature in the enamel reaction kettle to be 50 ℃ by using circulating water in the process until the epoxy chloropropane and the 40 percent dimethylamine aqueous solution are completely dropwise added, adding water-soluble chitosan with the deacetylation degree of 60 percent into the enamel reaction kettle, continuously stirring for 2 hours, and stopping the reaction to obtain the flocculant finished product.
The following are the laboratory pilot scale experiments and industrial production application effects of the environment-friendly flocculant (EEDC) of the present invention:
the environmental-friendly flocculant (EEDC) and CA of the invention have stability, coagulation effect and influence on performances of styrene butadiene rubber products, and are subjected to laboratory comparative experiments:
firstly, experimental conditions:
1) SBR No. 1502500 base latex is adopted; base solution: 500g of dry glue/10L of water; the coagulation temperature is 60 ℃; the pH value is 2.6;
2) evaluation samples: EDDC; the solid content was 50%.
And (3) comparison: CA; the solids content was 56%.
3) The addition amount is as follows: EDDC adding amount is 1.54 per mill and 1.68 per mill, CA adding amount is 2.2 per mill and 2.4 per mill;
second, experimental results
1) EDDC is steady in state during the configuration process (50% configured at 13.0%).
2) The results of the coagulation experiments are given in the following table
3) The effect of the samples on the properties of the styrene-butadiene rubber products is shown in the following Table
Thirdly, experimental conclusion: the EEDC has good flocculation effect, can achieve better flocculation effect when added according to 70 percent of CA dosage, and the service performance can reach the design requirement.
The laboratory comparative experiment of the environment-friendly flocculant (EEDC) of the present invention was thus completed.
Putting the environment-friendly flocculant (EEDC) into a styrene butadiene rubber production line of a certain factory for production test:
first, test conditions
1) Variety: SBR1502 brand
2) Production load: 145T/D
3) Controlling the conversion rate: 62 +/-2%
4) The production formula comprises: monomer ratio: 70.75/29.25
Soap/terminator: 97/230
Feeding level: 115 percent of
A regulator: 0.163
Second, testing procedure and Effect
1) The environment-friendly flocculating agent (EEDC) is prepared according to the preparation method and the raw material proportion, 200kg of the flocculant is barreled for standby, the appearance color is normal by visual inspection, no impurities exist, and the gas in the collection barrel is detected without formaldehyde components.
2) The method is carried out according to a conventional process, the production addition amount is 80L/h, about 60 percent of CA consumption and lower than 70 percent of expected consumption value, the cost per ton of the flocculant using EEDC as styrene butadiene rubber is saved by 1.48 yuan, the cost is basically equivalent to that of CA, gas on an operation site is collected for detection, and no formaldehyde component exists.
3) As the sewage of the three production lines of the test factory is collected to be produced by a single line, the test factory provides one production line. Before the test, CA is used as a flocculating agent in all three production lines, and sewage is collected to detect that the COD content is 800 PPM; in the test period, CA is used as a flocculating agent in two production lines, EEDC is used as a flocculating agent in one production line, and sewage is collected to detect that the COD content is 700 PPM; the COD content is obviously reduced.
4) The use of EEDC as a flocculant did not affect the drying of the coagulated size.
5) The impact of using EEDC as a flocculant on the quality of the finished gum is: the indexes of volatile matters, organic acids and the like of SBR 1502-brand products are all equivalent to those of finished glue using CA as a flocculating agent, wherein the stress value at 25 minutes of the finished glue using EEDC as the flocculating agent is higher than that of the finished glue using CA as the flocculating agent, and the quality of the finished product is improved.
The production test of the environment-friendly flocculant (EEDC) of the invention is finished.
And III, putting the environment-friendly flocculant (EEDC) into a butadiene styrene rubber device of a certain plant to perform a total nitrogen content in sewage and equipment corrosion influence test, producing according to a conventional process, replacing the original flocculant CA with the EEDC, wherein the test period is a 30-day production period, the total nitrogen content in the sewage is sampled and inspected every day, and the result is shown in the following table.
And (4) conclusion: the total nitrogen content in the sewage of the styrene butadiene rubber device is obviously reduced, the device is stable in production and operation during the test period, abnormal fluctuation does not occur, the main process parameters of the device are in the qualified range, and the operation stability rate is 100%; by 22 days after 4 months, 59 batches of SBR1500E brand finished product glue are produced, the total amount is 3144.43 tons, wherein 5 batches of finished product glue have no analysis structure, and other batches of finished product glue all meet the Q/SY1384-2011 high-class product standard; 63 batches of SBR 1502-brand finished product glue are produced, the total amount is 2853.575 tons, wherein 6 batches of finished product glue have no analysis result, 1 batch of finished product glue is qualified products with Mooney exceeding standard, and the rest batches of finished product glue all meet the GB12824-2002 high-class product standard; so far, butadiene styrene rubber products applying the environment-friendly flocculating agent (EEDC) are 122 batches, already 34 batches flow into the market, and no product defect feedback or quality complaint is received after tracking; no corrosion phenomenon of the equipment is found during the test, no other adverse effect is found, and the production requirement of the styrene butadiene rubber device can be met by using the environment-friendly flocculating agent (EEDC) in the aspects of reducing the total nitrogen of sewage, product physical index and production control.
So far, the total nitrogen content and equipment corrosion influence test of the environment-friendly flocculant (EEDC) is finished.
Claims (3)
1. The environment-friendly flocculant is characterized by being prepared from the following raw materials in parts by weight: 520-540 parts of epoxy chloropropane, 590-610 parts of dimethylamine aqueous solution with the concentration of 40%, 500-520 parts of pure water, 22-26 parts of water-soluble chitosan with the deacetylation degree of 60%, 23-27 parts of isopropanol and 1.8-2.2 parts of phosphorous acid catalyst.
2. The environment-friendly flocculant according to claim 1, wherein the flocculant is prepared from the following raw materials in parts by weight: 530 parts of epichlorohydrin, 600 parts of dimethylamine aqueous solution with the concentration of 40%, 510 parts of pure water, 24 parts of water-soluble chitosan with the deacetylation degree of 60%, 25 parts of isopropanol and 2 parts of phosphorous acid catalyst.
3. The method for preparing the environment-friendly flocculant according to claim 1 or 2, characterized by comprising the steps of:
1) adding 360 parts of pure water and a dimethylamine aqueous solution with the concentration of 40 percent into an enamel reaction kettle, adding isopropanol and a phosphorous acid catalyst, and controlling the internal vacuum degree of the reaction kettle to be 0.04 MPa-0.06 MPa;
2) preparing a metering tank A and a metering tank B, sucking epoxy chloropropane into the metering tank A in vacuum for standby, and sucking the dimethylamine aqueous solution with the residual concentration of 40% into the metering tank B in vacuum for standby;
3) starting an enamel reaction kettle to stir continuously under normal temperature environment, dropwise adding 45-50 parts per hour, dropwise adding epoxy chloropropane into the enamel reaction kettle through a metering tank A, dropwise adding 25-35 parts per hour, dropwise adding a dimethylamine aqueous solution with the concentration of 40% into the reaction kettle through a metering tank B, controlling the temperature in the reaction kettle to be 46-50 ℃ by using circulating water until the epoxy chloropropane and the dimethylamine aqueous solution with the concentration of 40% are completely dropwise added, adding water-soluble chitosan with the deacetylation degree of 60% into the reaction kettle, continuously stirring for 2 hours, stopping reaction, and obtaining a flocculant finished product.
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| CN105084480A (en) * | 2015-07-21 | 2015-11-25 | 安徽江威精密制造有限公司 | Wastewater flocculant and preparation method therefor |
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| CN101821273A (en) * | 2007-08-16 | 2010-09-01 | 富士胶片株式会社 | Heterocyclic compound, ultraviolet ray absorbent, and composition comprising the ultraviolet ray absorbent |
| CN103724460A (en) * | 2012-10-15 | 2014-04-16 | 中国石油化工股份有限公司 | Nitrile butadiene rubber latex coagulation technology |
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