CN102311140A - Method for simultaneously preparing recycling zinc carbonate and hydrochloric acid by chemical fiber waste residue mud - Google Patents
Method for simultaneously preparing recycling zinc carbonate and hydrochloric acid by chemical fiber waste residue mud Download PDFInfo
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- CN102311140A CN102311140A CN201110110707A CN201110110707A CN102311140A CN 102311140 A CN102311140 A CN 102311140A CN 201110110707 A CN201110110707 A CN 201110110707A CN 201110110707 A CN201110110707 A CN 201110110707A CN 102311140 A CN102311140 A CN 102311140A
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- hydrochloric acid
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Abstract
The invention belongs to the technical field of chemical industry three-waste treatment and utilization, and in particular relates to a method for simultaneously preparing recycling zinc carbonate and hydrochloric acid by chemical fiber waste residue mud. The main technical scheme comprises washing chemical fiber waste residue mud, preparing into diluted emulsion, reacting with hydrochloric acid, and recycling the gas generated during reaction after absorption; adding a small amount of calcium chloride and zinc hydroxide sequentially in the mixed liquid generated after reaction, and filtering after reaction; then carrying out reaction on filtrate and carbon dioxide to produce zinc carbonate and hydrochloric acid solution, and filtering; and washing filter cake, drying and crushing, checking weight and packaging to obtain a zinc carbonate powder product, and recycling the filtrate after concentration. According to the invention, not only is waste mud generated by the chemical fiber production industry treated effectively, the chemical industry pollution is eliminated, but also the chemical fiber waste mud can be changed into zinc carbonate and hydrochloric acid products with economic value, the production process and the device thereof are simple, and the cost is low.
Description
Technical field
The invention belongs to the technical field of three chemical wastes and utilization, especially a kind ofly prepare zinc carbonate co-production of hydrochloric cyclic utilization method with the chemical fibre waste dregs mud.
Technical background
Fiber is the requisite of social production and life, is the basic material of textile industry.What of kinds of fibers and quantity, the height of quality is the important symbol of production, science and technology and the standard of living height of a country.Current society, kinds of fibers is summarized to be divided into and is planted fibre, moving fibre and chemical fibre three major types; Man-made fiber is the product of modern industry development; Man-made fiber is to use the macromolecular compound of natural high moleculer eompound or synthetic to be raw material, through operation fibers that make, that have textile performance such as preparation spinning solution, spinning and aftertreatments; Whole world chemical fibre output was inclined more than 100 ten thousand tons in 1985; Account for the half the of three big fiber total amounts; Development along with petrochemical industry; The kind and the quantity of chemical fibre rise rapidly, and are widely used in making clothing fabric, filter cloth, travelling belt, rotary hose, rope, fishing net, electric insulated, medical suture, tire fabric and parachute etc.
And the preparation of man-made fiber is normally earlier processed spinning melt or solution to natural or synthetic polymer substance or inorganics, then through filtering, measuring, is extruded as liquid thread by spinning nozzle (plate), then solidifies to form fiber.The fiber of this moment is called nascent fibre, and its mechanical property is very poor, also must just can meet weaving processing and request for utilization through a series of post-treatment operations.The post-treatment operation is primarily aimed at that fiber stretches and thermal-setting, operations such as improving the mechanical property and the dimensional stability of fiber, the post-treatment of wet spun fibre also comprises washing, oils, drying.
In the post-treatment operation of artificial production of chemical fibre, need use a large amount of zinc sulfate (be commonly called as white vanadium and also be almagrerite) usually; When post-treatment, the zinc in the zinc sulfate does not finally get in the artificial man-made fiber, but all gets in the waste dregs mud, discharges along with waste water, and the waste water that receives zinc pollution must pass through purification and could discharge, and its throw out is the chemical fibre waste dregs mud.Since along with the quick growing trend of holding of chemical fibre requirement, produce chemical fiber waste water that chemical fibre produces and also increase year by year, all kinds of waste water that produce in the chemical fibre production process, the chemical fiber waste water complicated component often contains all kinds of toxic substances, and biodegradability is poor.Therefore at present, people have carried out big quantity research to the processing of waste water, for example: the Zhou Xiufeng of University Of Science and Technology Of Tianjin's ocean science and engineering college, interim " chemical engineering abstracts " 2007 the 4th, just method for treating wastewater of chemical fiber is summarized; But people study but seldom to the utilization again of waste dregs mud.
According to the statistics of the FSU to 12 chemical fibre factories, it is 15～40% that the zinc content in the waste dregs mud that 4 factories discharge is arranged, and the zinc content that all the other 8 factories discharge in waste dregs muds is 4～10%.So its zinc content on average carries out according to following ratio; And other components contents are following: zinc content is 38.4%, sulphur 2.73%, the sulphur 0.87% in the sulfide, total sulfur content 3.6% in the vitriol, iron level 1.1%, quicklime 0.3%, Natural manganese dioxide 0.25%.
The method of conventional process waste dregs mud normally press filtration becomes cake to transport accumulation, promptly is unfavorable for environmental protection, also wastes trucking costs, has especially wasted contained valuable material element in the waste dregs mud; Chemical fibre waste dregs mud yet of no use prepares the relevant report of the method for zinc carbonate co-production of hydrochloric at present.
Summary of the invention
The invention provides a kind of not only with low cost, be easy to realize that and technology and production unit simply prepare the method for zinc carbonate co-production of hydrochloric with the chemical fibre waste dregs mud.
In order to reach above-mentioned purpose, technical scheme of the present invention is:
A kind ofly prepare zinc carbonate co-production of hydrochloric cyclic utilization method, comprise being prepared as follows step with the chemical fibre waste dregs mud:
Steps A, the chemical fibre waste dregs mud is delivered to washing tank, with clear water the chemical fibre waste dregs mud is washed earlier, then chemical fibre waste dregs mud furnishing chemical fibre waste dregs mud dilute emulsion is being sent in first corrosion-resistant reactor;
Dropping into hydrochloric acid soln in step B, past first corrosion-resistant reactor reacts; Reaction generates zinc chloride and vitriolic mixed solution I; And carbonic acid gas and hydrogen sulfide, the mass ratio of chemical fibre waste dregs mud dilute emulsion and hydrochloric acid soln is 1: 0.74 in said first corrosion-resistant reactor; Utilize again after other absorptions of reaction gained;
Step C, the mixed solution I of gained among the step B is filtered with first strainer, filter cake impurity is buried or burn;
Step D, gained filtrating among the step C is transferred in second corrosion-resistant reactor, then adds calcium chloride in second corrosion-resistant reactor and react, reaction generates the mixed solution I I of calcium sulfate;
Step e, the mixed solution I I of gained among the step D is filtered with second strainer, filtering the clear filtrate that obtains is zinc chloride and a spot of hydrochloric acid mixed solution III, and filter cake impurity is buried or burn;
Step F, gained mixed solution I II in the step e is transferred in the 3rd corrosion-resistant reactor, then adds zinc hydroxide in the 3rd corrosion-resistant reactor and react, make mixed solution I V;
Step G, the mixed solution I V of gained in the step F filtered with the 3rd strainer obtain clarifying liquor zinci chloridi, filter cake impurity is buried or burn;
Step H, the liquor zinci chloridi of gained among the step G is transferred to earlier in the 4th corrosion-resistant reactor; React toward the interior carbonic acid gas that feeds of the 4th corrosion-resistant reactor then; Obtain the reaction mixture V of zinc carbonate and hydrochloric acid, the mass ratio of described liquor zinci chloridi and carbonic acid gas is 1: 0.32 in the 4th corrosion-resistant reactor;
Step I, the reaction mixture V of gained among the step H is filtered with the 4th strainer;
Step J, the filter cake of gained among the step I is washed drying, drying, pulverizes back jin inspection and be packaged to be the zinc carbonate product with washer, moisture eliminator, kibbler successively; Obtaining hydrochloric acid after filtrating concentrates with thickener returns among the step B.
Preferably, the waste dregs mud of chemical fibre described in steps A dilute emulsion is that solid content is 40% dilute emulsion.
Preferably, hydrochloric acid soln described in the step B is that volume percent is 26% hydrochloric acid soln.
The present invention utilizes chemical fibre waste dregs mud (mainly being alkali formula zinc hydroxide) washing back furnishing dilute emulsion and hydrochloric acid are reacted, and the gas that reaction generates utilizes through after absorbing again; The mixing liquid that reaction generates adds a little calcium chloride and zinc hydroxide successively; React after-filtration; To filtrate then and react with carbonic acid gas; Produce zinc carbonate and hydrochloric acid soln, filter the back filter cake wash, dry, checking the weight after pulverizing is packaged to be the zinc carbonate powder product, hydrochloric acid filtrating concentrates the back recycle; The present invention has not only effectively administered the useless mud that the chemical fibre production industry is produced, and eliminates chemical pollution, and can the chemical fibre waste dregs mud be transformed into the zinc carbonate and the salt acid product of economically valuable, and production technique and equipment thereof are simple, and is with low cost.
Its chemical equation is following: Zn (OH)
2+ 2HCl====ZnCl
2+ 2H
2O
ZnCl
2+CO
2+H
2O＝＝＝＝ZnCO
3+2HCl
The impurity and purification equation is following: H
2SO
4+ CaCl
2====CaSO
4+ 2HCl
2HCl+Zn(OH)
2＝＝＝＝ZnCl
2+2H
2O
Description of drawings
Fig. 1 is the process flow diagram for preparing the zinc carbonate co-production of hydrochloric with the chemical fibre waste dregs mud,
Wherein:
The 1-washing tank, 2-first corrosion-resistant reactor, 3-first strainer, 4-second corrosion-resistant reactor; 5-second strainer, 6-the 3rd corrosion-resistant reactor, 7-the 3rd strainer, 8-the 4th corrosion-resistant reactor; 9-the 4th strainer, 10-washer, 11-moisture eliminator; The 12-kibbler, 13-zinc carbonate product, 14-thickener.
Concrete embodiment
A kind ofly prepare zinc carbonate co-production of hydrochloric cyclic utilization method, comprise being prepared as follows step with the chemical fibre waste dregs mud:
Steps A, 1000kg chemical fibre waste dregs mud is delivered to washing tank 1, with clear water the chemical fibre waste dregs mud is washed earlier, washing back furnishing solid content is to be sent in first corrosion-resistant reactor 2 behind 40% the chemical fibre waste dregs mud dilute emulsion; Wherein, contain zinc hydroxide 384kg in the chemical fibre waste dregs mud, contain sulfide 36kg;
Dropping into hydrochloric acid solns (concentration of volume percent is 26%) in step B, past first corrosion-resistant reactor 2 reacts; Reaction generates zinc chloride and vitriolic mixed solution I; And carbonic acid gas and hydrogen sulfide, the mass ratio of chemical fibre waste dregs mud dilute emulsion and hydrochloric acid soln is 1: 0.74 in said first corrosion-resistant reactor 2;
Step C, the mixed solution I of gained among the step B is filtered with first strainer 3, filter cake impurity is buried or burn;
Step D, gained filtrating among the step C is transferred in second corrosion-resistant reactor 4; Then react toward second corrosion-resistant reactor, the 4 interior calcium chloride that add; Reaction generates the mixed solution I I of calcium sulfate; (adding calcium chloride is to form deposition in order to remove unnecessary sulfuric acid molecule, and the addition of calcium chloride can draw based on the cubage of sulphur in the waste dregs mud);
Step e, the mixed solution I I of gained among the step D is filtered with second strainer 5, filtering the clear filtrate that obtains is zinc chloride and a spot of hydrochloric acid mixed solution III, and filter cake impurity is buried or burn;
Step F, gained mixed solution I II in the step e is transferred in the 3rd corrosion-resistant reactor 6; Then react toward the 3rd corrosion-resistant reactor 6 interior zinc hydroxides that add; Make mixed solution I V; (add a spot of zinc hydroxide and be in order to make unnecessary hydrochloric acid form liquor zinci chloridi again, liquor zinci chloridi concentration is increased and removed chloride impurity simultaneously, the add-on of zinc hydroxide can calculate according to the amount that adds hydrochloric acid that calcium chloride produces);
Step G, the mixed solution I V of gained in the step F filtered with the 3rd strainer 7 obtain clarifying liquor zinci chloridi, filter cake impurity is buried or burn;
Step H, the liquor zinci chloridi of gained among the step G is transferred to earlier in the 4th corrosion-resistant reactor 8; React toward the 4th corrosion-resistant reactor 8 interior carbonic acid gas that feed then; Obtain the reaction mixture V of zinc carbonate and hydrochloric acid, the mass ratio of described liquor zinci chloridi and carbonic acid gas is 1: 0.32 in the 4th corrosion-resistant reactor 8;
Step I, the reaction mixture V of gained among the step H is filtered with the 4th strainer 9;
Step J, the filter cake of gained among the step I is washed drying, drying, pulverizes back jin inspection and be packaged to be 491.50kg zinc carbonate product 13 with washer 10, moisture eliminator 11, kibbler 12 successively; Obtaining 285.77kg hydrochloric acid after filtrating concentrates with thickener 14 returns among the step B.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting practical range of the present invention, so all equivalences of being done with described characteristic of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (3)
1. one kind prepares zinc carbonate co-production of hydrochloric cyclic utilization method with the chemical fibre waste dregs mud, it is characterized in that: comprise being prepared as follows step:
Steps A, the chemical fibre waste dregs mud is delivered to washing tank, with clear water the chemical fibre waste dregs mud is washed earlier, then chemical fibre waste dregs mud furnishing chemical fibre waste dregs mud dilute emulsion is being sent in first corrosion-resistant reactor;
Dropping into hydrochloric acid soln in step B, past first corrosion-resistant reactor reacts; Reaction generates zinc chloride and vitriolic mixed solution I; And carbonic acid gas and hydrogen sulfide, the mass ratio of chemical fibre waste dregs mud dilute emulsion and hydrochloric acid soln is 1: 0.74 in said first corrosion-resistant reactor; Utilize again after other absorptions of reaction gained;
Step C, the mixed solution I of gained among the step B is filtered with first strainer, filter cake impurity is buried or burn;
Step D, gained filtrating among the step C is transferred in second corrosion-resistant reactor, then adds calcium chloride in second corrosion-resistant reactor and react, reaction generates the mixed solution I I of calcium sulfate;
Step e, the mixed solution I I of gained among the step D is filtered with second strainer, filtering the clear filtrate that obtains is zinc chloride and a spot of hydrochloric acid mixed solution III, and filter cake impurity is buried or burn;
Step F, gained mixed solution I II in the step e is transferred in the 3rd corrosion-resistant reactor, then adds zinc hydroxide in the 3rd corrosion-resistant reactor and react, make mixed solution I V;
Step G, the mixed solution I V of gained in the step F filtered with the 3rd strainer obtain clarifying liquor zinci chloridi, filter cake impurity is buried or burn;
Step H, the liquor zinci chloridi of gained among the step G is transferred to earlier in the 4th corrosion-resistant reactor; React toward the interior carbonic acid gas that feeds of the 4th corrosion-resistant reactor then; Obtain the reaction mixture V of zinc carbonate and hydrochloric acid, the mass ratio of described liquor zinci chloridi and carbonic acid gas is 1: 0.32 in the 4th corrosion-resistant reactor;
Step I, the reaction mixture V of gained among the step H is filtered with the 4th strainer;
Step J, the filter cake of gained among the step I is washed drying, drying, pulverizes back jin inspection and be packaged to be the zinc carbonate product with washer, moisture eliminator, kibbler successively; Obtaining hydrochloric acid after filtrating concentrates with thickener returns among the step B.
2. according to claim 1ly prepare zinc carbonate co-production of hydrochloric cyclic utilization method with the chemical fibre waste dregs mud, it is characterized in that: the waste dregs mud of chemical fibre described in steps A dilute emulsion is that solid content is 40% dilute emulsion.
3. according to claim 1ly prepare zinc carbonate co-production of hydrochloric cyclic utilization method with the chemical fibre waste dregs mud, it is characterized in that: hydrochloric acid soln described in the step B is that volume percent is 26% hydrochloric acid soln.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115446096A (en) * | 2022-08-29 | 2022-12-09 | 北京科技大学 | Method for preparing blast furnace injection fuel and zinc carbonate by cracking waste tire carbon black |
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2011
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115446096A (en) * | 2022-08-29 | 2022-12-09 | 北京科技大学 | Method for preparing blast furnace injection fuel and zinc carbonate by cracking waste tire carbon black |
| CN115446096B (en) * | 2022-08-29 | 2023-08-08 | 北京科技大学 | Method for preparing blast furnace injection fuel and zinc carbonate by cracking carbon black from waste tires |
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Application publication date: 20120111 |