CN102337164B - Method for processing waste water from production device of vulcanization accelerator - Google Patents
Method for processing waste water from production device of vulcanization accelerator Download PDFInfo
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- CN102337164B CN102337164B CN201010238857.9A CN201010238857A CN102337164B CN 102337164 B CN102337164 B CN 102337164B CN 201010238857 A CN201010238857 A CN 201010238857A CN 102337164 B CN102337164 B CN 102337164B
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Abstract
The invention relates to a method for processing waste water from a production device of a vulcanization accelerator, which is characterized in that the method comprises the following steps: weighting waste water of a vulcanization accelerator CBS, adding a sulfonating agent, stirring and dissolving; heating, adding a ketone compound into waste liquid, sulfonating under the stirring condition; heating a reaction system, adding an aldehyde compound for reacting; adding the reaction product in waste water from the vulcanization accelerator CBS, continuously reacting to prepare a coal water slurry additive solution. On one hand, the method is capable of effectively solving the problems of discharge and treatment of chemical waste water and minimizing the environmental pollution caused by organic waste water. On the other hand, the method of the invention is capable of reducing the cost of the coal water slurry and realizing the purpose of changing waste into valuables.
Description
Technical field
The present invention relates to waste water treatment process, be specially a kind of method of processing vulcanization accelerator production equipment waste water,, by utilizing polymer chemistry reaction to prepare a technology for slurries additive agent in waste water, be espespecially a kind of method of utilizing vulcanization accelerator production equipment waste water to prepare slurries additive agent.
Background technology
Chemical industry is the traditional mainstay industry of China, and industrial chemicals and product that the sector is produced are widely used in national defence, the fields such as medicine and agricultural chemicals.Along with chemical industry production technology and throughput improve constantly, the wastewater discharge that produced is in process of production also constantly soaring.How processing a large amount of waste water that produce is in process of production focuses that current chemical enterprise is paid close attention to.Traditional method of wastewater treatment has biochemical treatment, film is processed etc., yet in the waste water that most of chemical enterprise discharges, contains a large amount of organic compound, this class chemistry of organic compound stable in properties, the more difficult method of processing by biochemistry and film is processed, and waste water is difficult to reach emission standard.
The waste water that the production equipment that the vulcanization accelerator CBS that Nan Hua company produces adopts produces is the poisonous and hazardous compound of difficult degradation mostly.It is large that this strand of vulcanization accelerator CBS waste water has the water yield, and the features such as organic contamination substrate concentration is high, colourity dark, alkalescence is large, complicated component, belong to unmanageable trade effluent.The pH of this waste water is 11 left and right, COD
crbe 1000～100000, in waste water, contain a large amount of organism, hard degradation.Treatment process for this class waste water is to burn and chemical method up to now, and these treatment process investments are large, and treating processes is unstable, is difficult to qualified discharge.
Coal water slurry is a kind of pulverized coal particle by 60%-70% left and right, the coal-based liquid fuel that the additive of the water of 30%-40% left and right and 1%-1.5% left and right is prepared from through physical mixed.Have the same mobility and the stability of image-stone oil, combustion heat value is high.China has abundant coal resources deposit, in short supply along with petroleum-based energy, and coal water slurry gets more and more people's extensive concerning as a kind of good energy substitution product.
Due to the uncompatibility of water and coal, in the preparation process of coal water slurry, in mixture, add chemical additive, as dispersion agent, stablizer and other auxiliary agents improve mobility and the stability in storage of coal water slurry.Dispersion agent is important a kind of in slurries additive agent, is mainly to take tensio-active agent as main, can be divided into anionic and non-ionic type.Aniorfic surfactant comprises sulfonate, carboxylate salt and a small amount of phosphoric acid ester, and generally application is sulfonate, as sulfonated lignin and sulfonated petro-leum etc.Nonionic surface active agent mainly contains polyoxyethylene series and polyoxy ethane series.Although non-ionic type surface additive is effective, preparation cost is high, is unsuitable for scale operation.
In recent years, with papermaking wastewater or trade effluent, preparing coal water slurry is also widely reported.As utilize slurries production technology to process the method (Chinese patent application 200710026686 of textile printing and dyeing wastewater, notification number CN100486917C), a kind of environment protection type coal water slurry and method for making thereof (application number: 200810079340.2, notification number: CN101440317A), a kind of coal water slurry dispersing and preparation method thereof (Chinese patent application 200810029825.0, notification number CN101322927A) etc., adopt such technical finesse waste water not only to reduce the cost of coal water slurry, and solved the exhaust emission environmental problem of waste water, but also do not realize and utilize wastewater from chemical industry to prepare slurries additive agent so far.
Document 1 (Zhou Mingsong etc., fine chemistry industry, 2005, No.22 (3): 185-188) reported the synthesis technique of slurries additive agent sulphonated acetone formaldehyde polycondensates in pure water, yet also do not realized and prepare this base polymer in wastewater from chemical industry now.
Summary of the invention
The technical problem to be solved in the present invention:
The shortcoming existing for prior art, the object of the present invention is to provide a kind of method of processing vulcanization accelerator CBS waste water, at waste water, utilize solution polymerization to prepare slurries additive agent in mutually, avoid vulcanization accelerator CBS discharge of wastewater to the environment produced pollution, realized the useless Water reuse of vulcanization accelerator CBS.
Vulcanization accelerator CBS waste water of the present invention refers to the waste water of vulcanization accelerator production equipment (for example Nan Hua company), wherein contains a large amount of organism, and the feature of water is as shown in the table:
The technical scheme that the present invention takes is:
A method of processing vulcanization accelerator CBS waste water, comprises the steps:
Step 1: take above-mentioned 50 parts of vulcanization accelerator CBS waste water (mass ratio), add 2～5 parts of sulphonating agents, stirring and dissolving;
Step 2: be warming up to 40～60 ℃, in this waste liquid, add 3～7 parts of ketone compounds, sulfonation under agitation condition, the sulfonation time is 30～60 minutes;
Step 3: reaction system is warming up to 70～90 ℃, evenly adds the aldehyde compound of 3～10 parts in 0.5h～2h, ketone compounds and aldehyde compound reaction 1～5h at this temperature;
Step 4: reaction product (slurries additive agent) is joined in the vulcanization accelerator CBS waste water of 400～800 parts, continue reaction 1～2h, make slurries additive agent solution.
Described slurries additive agent, its raw material in mass, is filled a prescription as follows: 50 parts of vulcanization accelerator CBS waste water; 3～7 parts of ketone compounds (as acetone); 3～10 parts of aldehyde compounds; 2～5 parts of sulphonating agents; Screening formulation is 50 parts of vulcanization accelerator CBS waste water; 5 parts, acetone; 3.5～7 parts of aldehyde compounds; 2～5 parts of sulphonating agents.
Described sulphonating agent can be following one or more: S-WAT, Sodium Pyrosulfite and sodium bisulfite, when appointing, to get above multiplely while making composite sulphonating agent, and proportioning can be selected arbitrarily.
Described ketone compounds can be following one or more: acetone, cyclohexanone analog compound, when to choose ketone compounds be multiple, proportioning is any.
Described aldehyde compound is one or more in following: formaldehyde, acetaldehyde, propionic aldehyde, oxalic dialdehyde and glutaraldehyde, when aldehyde is when to choose compounds be multiple, proportioning is any.
Preferred version is that described sulphonating agent is S-WAT; Described ketone compounds is acetone; Described aldehyde compound is formaldehyde.
The present invention is directed to vulcanization accelerator CBS waste water, first in this waste water, prepare slurries additive agent, again slurries additive agent and non-caking coal slurrying are obtained to coal water slurry, proportioning raw materials and reaction conditions have been optimized, and utilize the active principle in vulcanization accelerator CBS waste water to participate in reaction, improve reaction efficiency.
Compare with the report of document 1, the present invention utilizes vulcanization accelerator CBS waste water as solvent, adjusted different components (S-WAT in polymerization process, formaldehyde, acetone) proportioning, and sulfonation temperature and temperature of reaction are optimized, and utilize the reactive behavior of organic constituent in waste water to make it participate in polyreaction, play the effect of utilization of waste material.
The improvement of the method for the present invention and document 1 report is:
(1) the present invention's waste water used is alkaline waste water, and wherein the existence of contained hydroxide ion exists promoter action to polyreaction, and in waste water, the contained inorganic salt such as NaCl can play stabilization to the coal water slurry preparing.Therefore, the present invention utilizes hydroxide ion and the NaCl in waste water, has improved reaction efficiency on the one hand, has saved on the other hand the step of preparing composite inorganic salt stablizer in slurries additive agent process, has saved cost;
(2) to prepare proportioning and the reaction conditions of sulphonating agent, acetone and formaldehyde in slurries additive agent process in waste water, improve and optimize, as solvent phase ratio, great changes have taken place for the optimum amount of various reaction reagents with pure water;
(3) in the present invention's waste water used, contained effective constituent can participate in polymerization, and the molecular weight of resulting additive can be by controlling reacting material ratio, and reaction times and sulfonation temperature are controlled;
With slurry by this invention formulation additives and non-caking coal are carried out, the additive that proves this kind has good dispersion and falls glutinous usefulness, and the slurry stability making is good.Because non-caking coal belongs to the coal of difficult slurrying, therefore measurable this additive is applicable to the coal slurrying of different rank.
The invention has the beneficial effects as follows:
The method of processing vulcanization accelerator CBS waste water of the present invention, utilize this waste water as solvent, utilize therein ketone and aldehydes to react to prepare slurries additive agent, efficiently solve on the one hand the discharge of this type of wastewater from chemical industry and administer a difficult problem, reduced the pollution of organic waste water to environment.Also reduce on the other hand the cost of coal water slurry, realized the object turning waste into wealth, and reduced investment and the working cost of processing waste water, there is obvious economic and social benefit.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of embodiment 1 products therefrom.
Fig. 2 is the molecular weight distribution of embodiment 2 products therefroms.
Embodiment
Embodiment 1:
The vulcanization accelerator CBS waste water of Qu50gNan Hua company (pH 12, COD 30000mg/L, hexahydroaniline 20000mg/L, 2-mercaptobenzothiazole 1000mg/L) joins in there-necked flask, adds wherein 3g S-WAT, stirring and dissolving;
Be warming up to 40 ℃, add 5g acetone, under agitation sulfonation 30min;
Reaction system is warming up to 80 ℃, and the formaldehyde solution that is 37% by 10g concentration in 0.5h adds, and continues reaction 2h;
This product is joined in 400g vulcanization accelerator CBS waste water, continue reaction 1h, make slurries additive agent solution.
The infrared spectrum of products therefrom as shown in Figure 1.
Non-caking coal is passed through to ball mill grinding, obtain the coal dust that mass percent that median size is less than the particle of 75 μ m is greater than 80%, after the slurries additive agent solution obtaining and non-caking coal coal dust are mixed according to mass ratio preparation in 38: 62, by electric blender, stir and within 10 minutes, obtain coal water slurry.When the additive capacity of this coal water slurry is 1.0%, slurrying concentration is 62%, and the slurrying mobility of this coal water slurry is better, places 10 days, a small amount of bleed, soft precipitation.
Embodiment 2:
The vulcanization accelerator CBS waste water of Qu50gNan Hua company (pH 11, COD 20000mg/L, hexahydroaniline 559mg/L, 2-mercaptobenzothiazole 2000mg/L) joins in there-necked flask, adds wherein 2g S-WAT, stirring and dissolving;
Be warming up to 40 ℃, add 5g acetone, under agitation sulfonation 30min;
Reaction system is warming up to 85 ℃, and the formaldehyde solution that is 37% by 15g concentration in 0.5h adds, and continues reaction 2h;
This product is joined in 400g vulcanization accelerator CBS waste water, continue reaction 1h, make slurries additive agent solution.
As shown in Figure 2, molecular weight distribution is wider for the molecular weight distribution of product, mainly concentrates on 10000 left and right.
Hexahydroaniline content in solution is measured, and the hexahydroaniline content of CBS waste water is 5591mg/L, and in waste water, carrying out after polymerization measurement ring hexylamine content is again 52.4mg/L, illustrates that most of hexahydroaniline has all participated in reaction in reaction process.
Non-caking coal is passed through to ball mill grinding, obtain the coal dust that mass percent that median size is less than the particle of 75 μ m is greater than 80%, after the slurries additive agent obtaining and non-caking coal coal dust are mixed according to mass ratio preparation in 38: 62, by electric blender, stir and within 10 minutes, obtain coal water slurry.When the additive capacity of this coal water slurry is 1.0%, slurrying concentration is 62%, and the slurrying mobility of this coal water slurry is better, places 10 days, a small amount of bleed, soft precipitation.
Embodiment 3:
The vulcanization accelerator CBS waste water of Qu50gNan Hua company (pH 13, COD 80000mg/L, hexahydroaniline 60000mg/L, 2-mercaptobenzothiazole 15000mg/L) joins in there-necked flask, adds wherein 5g S-WAT, stirring and dissolving;
Be warming up to 60 ℃, add 7g acetone, under agitation sulfonation 60min;
Reaction system is warming up to 90 ℃, and the formaldehyde solution that is 37% by 15g concentration in 1h adds, and continues reaction 5h;
This product is joined in 400g vulcanization accelerator CBS waste water, continue reaction 2h, make slurries additive agent solution.
Non-caking coal is passed through to ball mill grinding, obtain the coal dust that mass percent that median size is less than the particle of 75 μ m is greater than 80%, after the slurries additive agent obtaining and non-caking coal coal dust are mixed according to mass ratio preparation in 38: 62, by electric blender, stir and within 10 minutes, obtain coal water slurry.When the additive capacity of this coal water slurry is 1.0%, slurrying concentration is 62%, and the slurrying mobility of this coal water slurry is better, places 10 days, a small amount of bleed, soft precipitation.
By the known slurries additive agent of molecular weight distribution, when obtaining good dispersion effect, range of molecular weight distributions is 2000～30000.
Claims (6)
1. a method of processing vulcanization accelerator CBS waste water, comprises the steps:
Step 1: take 50 parts of above-mentioned vulcanization accelerator CBS waste water, add 2～5 parts of sulphonating agents, stirring and dissolving;
Step 2: be warming up to 40～60 ℃, in this waste liquid, add 3～7 parts of ketone compounds, sulfonation under agitation condition, the sulfonation time is 30～60min;
Step 3: reaction system is warming up to 70～90 ℃, evenly adds the aldehyde compound of 3～10 parts in 0.5h～2h, ketone compounds and aldehyde compound reaction 1～5h at this temperature;
Step 4: reaction product is joined in the vulcanization accelerator CBS waste water of 400～800 parts, continue reaction 1～2h, make slurries additive agent solution;
Described sulphonating agent can be following one or more: S-WAT, Sodium Pyrosulfite and sodium bisulfite, when appointing, to get above multiplely while making composite sulphonating agent, and proportioning can be selected arbitrarily;
Described ketone compounds can be following one or more: acetone, cyclohexanone analog compound, and when to choose ketone compounds be multiple, proportioning is any;
Described aldehyde compound is one or more in following: formaldehyde, acetaldehyde, propionic aldehyde, oxalic dialdehyde and glutaraldehyde, and when aldehyde is when to choose compounds be multiple, proportioning is any;
Above-mentioned each umber is mass parts.
2. method according to claim 1, wherein adds 3.5～7 parts of aldehyde compounds in step 3.
3. method according to claim 1 and 2, wherein said sulphonating agent is S-WAT; Described ketone compounds is acetone; Described aldehyde compound is formaldehyde.
4. a slurries additive agent, its raw material in mass, is filled a prescription as follows: 50 parts of vulcanization accelerator CBS waste water; 3～7 parts of ketone compounds; 3～10 parts of aldehyde compounds; 2～5 parts of sulphonating agents
Described sulphonating agent can be following one or more: S-WAT, Sodium Pyrosulfite and sodium bisulfite, when appointing, to get above multiplely while making composite sulphonating agent, and proportioning can be selected arbitrarily;
Described ketone compounds can be following one or more: acetone, cyclohexanone analog compound, and when to choose ketone compounds be multiple, proportioning is any;
Described aldehyde compound is one or more in following: formaldehyde, acetaldehyde, propionic aldehyde, oxalic dialdehyde and glutaraldehyde, when aldehyde is when to choose compounds be multiple, proportioning is any.
5. slurries additive agent according to claim 4, its formula is 50 parts of vulcanization accelerator CBS waste water; 5 parts of ketone compounds; 3.5～7 parts of aldehyde compounds; 2～5 parts of sulphonating agents.
6. according to the slurries additive agent described in claim 4 or 5, wherein said sulphonating agent is S-WAT; Described ketone compounds is acetone; Described aldehyde compound is formaldehyde.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634794A (en) * | 2003-12-31 | 2005-07-06 | 吴霖秀 | High efficiency aliphatic sulfonate water reducing agent and method for preparing same |
| CN1818041A (en) * | 2006-03-08 | 2006-08-16 | 华南理工大学 | Hydrophilous slurry additive with mediben lignin and production thereof |
| CN101225336A (en) * | 2008-02-01 | 2008-07-23 | 福州大学 | Alkali lignin-sulphonated acetone formaldehyde polycondensates coal water slurry additive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634794A (en) * | 2003-12-31 | 2005-07-06 | 吴霖秀 | High efficiency aliphatic sulfonate water reducing agent and method for preparing same |
| CN1818041A (en) * | 2006-03-08 | 2006-08-16 | 华南理工大学 | Hydrophilous slurry additive with mediben lignin and production thereof |
| CN101225336A (en) * | 2008-02-01 | 2008-07-23 | 福州大学 | Alkali lignin-sulphonated acetone formaldehyde polycondensates coal water slurry additive and preparation method thereof |
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