CN103395816B - Process for producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle - Google Patents
Process for producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle Download PDFInfo
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Abstract
The invention relates to a process for producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle, and belongs to the technical field of waste liquor treatment in aramid fiber II production. The process comprises the following steps of: acid pickle pretreating, feeding, reacting and crystallizing, thickening, filtering, precipitating and the like. According to the invention, a problem that a process for treating acid pickle to recycle byproduct calcium sulphate dihydrate in the prior art cannot be directly used for treating the acid pickle generated in an aramid fiber II spinning process to recycle the byproduct calcium sulphate dihydrate due to different fields and different treated acid pickle is solved. The process for continuously producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle, provided by the invention, can be used for treating the acid pickle generated in the aramid fiber II spinning to efficiently produce calcium sulphate with high quality.
Description
Technical field
The present invention relates to the technique of liquid waste disposal and recycling in a kind of aramid II, more particularly, the present invention relates to a kind of technique utilizing aramid II spent acid solution to produce terra alba, belong to liquid waste disposal technique field in aramid II production.
Background technology
PPTA (PPTA) fiber is the very wide special fibre material of application prospect that 20 century 70s grow up, because it has high strength, high-modulus, resistant to elevated temperatures excellent properties, be applied widely at space flight, aviation, communication field, in national defense construction and the development of the national economy, occupy an important position, there is far-reaching influence and meaning.
In the production of aramid II, need in last spinning process to use acid bath, discarded dilute sulfuric acid solution can be produced, wherein for the task of bearing the useless dilution heat of sulfuric acid 50000 tons of process annual about 8% of Waste acid treating device.Because dilute sulphuric acid directly discharges severe contamination local environment, just can discharge after having to pass through governance for reaching standard, general treatment process, such as neutralization or concentrated, cost is higher, and the byproduct high less than economic worth produces, for rationally administering and utilizing this part waste acid resource, anxious to be studied go out a kind of can low-cost processes spent acid and the spent acid treatment process of high value byproduct can be produced.
Terra alba, i.e. gypsum, medium-to-high grade calcium sulfate is mainly used in the fields such as food, medicine, chemical industry, paint, beer fermentation, cement, edible mushrooms, granulation of fertilizer, foodstuff additive, chemical industry stopping composition.And the spent acid solution in the production technique of aramid II just can be used for remanufacture terra alba, improve salvage value, produce extra economic worth.
It is CN102275970A that State Intellectual Property Office discloses a publication number in 2011.12.14, and the patent of invention that name is called " titanium white waste acid wastewater utilization method ", which discloses a kind of titanium white waste acid wastewater utilization method, belong to field of metallurgy.The inventive method will to solve in prior art low cost can not make full use of the technical problem of titanium white waste acid waste water.Titanium white waste acid wastewater utilization method, comprises the following steps: a, in hydrochloric acid soln, add Wingdale, is fully obtained by reacting calcium chloride solution; B, in calcium chloride solution, add titanium white waste acid or waste water, fully filter to obtain terra alba and filtrate after reaction, the process of described terra alba drying obtains product gypsum; C, step b gained filtrate to be reacted as the raw material and Wingdale producing calcium chloride solution, after repeating step a and b is once above, in step b gained filtrate, add sodium hydroxide solution, fully filter the throw out obtaining sodium chloride solution and be rich in iron, titanium, vanadium, scandium and gallium after reaction.The inventive method is with low cost, can solve the problem of titanium white waste acid and waste water environmental pollution, has good promotion prospect.
Describe in above-mentioned patent in field of titanium dioxide production, mainly adopt Titanium White Production By Sulfuric Acid Process, the spent acid that Titanium White Production By Sulfuric Acid Process produces is referred to as titanium white waste acid, and the essential substance of titanium white waste acid consists of: sulfuric acid, iron, titanium, vanadium, scandium and gallium.And in the spinning process of aramid II, the spent acid solution that its acid bath produces mainly contains: content is the sulfuric acid of 6 ~ 10%; A small amount of oligopolymer and fracture of wire; The silicone oil of trace and iron, sodium, nickel ion; All the other are water.Although there is the technique utilizing the sulfuric acid in spent acid solution to prepare terra alba in prior art, but its technical field, composition in waste liquid and treatment process are not identical, the spent acid solution process produced in aramid II spinning process can not be directly used in, and cannot high quality, efficient, continuous print by-product terra alba.
Summary of the invention
The present invention is intended to solve the technique that by-product terra alba is reclaimed in spent acid solution process of the prior art, because field is different, the spent acid solution of process is different, the problem that by-product terra alba is reclaimed in the spent acid solution process produced in aramid II spinning process can not be directly used in, a kind of technique utilizing aramid II spent acid solution continuous seepage terra alba is provided, the spent acid solution that can produce for aramid II spinning, process, high quality, produce terra alba efficiently, not only refuse reclamation, and the higher product of economic worth can be produced.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
Utilize aramid II spinning spent acid solution to produce a technique for terra alba, it is characterized in that: comprise following processing step:
A, spent acid solution pre-treatment
Aramid II spinning spent acid solution is filtered by strainer, then through surge tank, the sulfuric acid concentration fluctuation range in the aramid II spinning spent acid solution described in control;
B, charging
Add in reactive crystallization device by steps A through pretreated aramid II spinning spent acid solution, in reactive crystallization device, add calcium carbonate slurry, the described sulfuric acid in pretreated aramid II spinning spent acid solution and the mol ratio between the calcium carbonate in coarse whiting are 1.02 ~ 1.12:1 simultaneously;
C, reactive crystallization
The mixing speed controlling reactive crystallization device is 150 ~ 200r/min, and adjusting process water flow velocity is 2 ~ 6m3/h, makes, through pretreated aramid II spinning spent acid solution and calcium carbonate slurry reactive crystallization, to obtain reactive crystallization slurry;
D, dense
The reactive crystallization slurry obtained by step C passes in dense device, carries out solid-liquid separation, improves the mass concentration of terra alba in reactive crystallization slurry;
E, filtration
Reactive crystallization slurry through dense device in step D is passed into vacuum band-type filter machine, filters;
F, precipitation
Slurry through filtering is inputed to settling tank precipitation, solid and liquid separation, the parting liquid obtained and precipitation, precipitation is product terra alba of the present invention.
Preferably, in step, the precision of described strainer is 150 ~ 250 orders in the present invention.
Preferably, in step, the volume of described surge tank is 8 ~ 12 times of described aramid II spinning spent acid solution generation volume per hour in the present invention.
Preferably, in stepb, the coarse whiting mass percent in described calcium carbonate slurry is 8 ~ 10% in the present invention, and wherein coarse whiting granularity is 150 ~ 200 orders, CaCO
3content>=95%, whiteness>=93%.
Preferably, in step D, in described raising reactive crystallization slurry, the mass concentration of terra alba refers to and the mass concentration of terra alba in reactive crystallization slurry is brought up to 35 ~ 45% in the present invention.
Preferably, the present invention is in step e, and the vacuum degree control of described vacuum band-type filter machine is-0.06 ~-0.08MPa, and the water content control through the reactive crystallization slurry of vacuum band-type filter machine filtration is≤22%, whiteness >=85%.
Preferably, the aramid II spinning spent acid solution that utilizes of the present invention is produced in the technique one-period of terra alba, after step F obtains terra alba by precipitation, the parting liquid part reuse obtained is to reactive crystallization, dense and filtration step, and another part is for preparing calcium carbonate slurry.
Further, described settling tank and described reactive crystallization device, by two communication, form inner cycle channel.
Further, the process water overflow in described dense device is to vacuum band-type filter machine and settling tank.
The Advantageous Effects that the present invention brings:
1, the invention solves the technique that by-product terra alba is reclaimed in spent acid solution process of the prior art, because field is different, the spent acid solution of process is different, the problem that by-product terra alba is reclaimed in the spent acid solution process produced in aramid II spinning process can not be directly used in, a kind of technique utilizing aramid II spent acid solution continuous seepage terra alba is provided, the spent acid solution that can produce for aramid II spinning, process, high quality, produce terra alba efficiently, not only refuse reclamation, and the higher product of economic worth can be produced.The useless diluted acid that the improvement aramid fiber of economical rationality is a large amount of.The method flow process is shorter, and equipment investment is less, simple to operate, is convenient to control, and turns waste into wealth, and reduce environmental protection treatment cost, energy consumption is lower.The present invention is in the step of charging and reaction, and by controlling suitable stirring velocity and process water flow velocity can make reaction carry out continuously and evenly, and be conducive to growing up of crystal grain, be beneficial to reaction and carry out continuously, calcium carbonate residual volume increases.So, by controlling inlet amount, stirring velocity and process water flow velocity, being controlled the reaction times is 2 ~ 3 hours, and crystallization control granularity is at 0.1 ~ 0.4mm, thus substantially increase the quality quantity of production efficiency and the finished product, the pH value that the control of above-mentioned inlet amount can also control when reacting is 6 ~ 8, improves the utilization ratio of the acid in spent acid, improves the rate of recovery and the quality of product.
2, the present invention is preferred, and the precision of strainer is in step 150 ~ 250 orders, can effectively remove oligopolymer and fracture of wire; The present invention is preferred, and in step, the volume of described surge tank is 8 ~ 12 times of described aramid II spinning spent acid solution generation volume per hour.The selection of the proportionlity between the volume of above-mentioned surge tank solvent and spent acid solution generation per hour can control the described concentration difference < 5% of aramid II spinning spent acid solution often between adjacent two hours, effectively can prevent the big ups and downs of spent acid solution concentration; And select surge tank to keep stable input little to concentration, without the need to adding power and other raw material.
4, the present invention is preferred, and in stepb, the coarse whiting mass percent in described calcium carbonate slurry is 8 ~ 10%, and wherein coarse whiting granularity is 150 ~ 200 orders, CaCO
3content>=95%, whiteness>=93%, and in reactive crystallization device, pH is 6 ~ 8.Above-mentioned carrying out smoothly of subsequent reactions crystallization is conducive to for the selection of pH in coarse whiting raw material standard and reactive crystallization device.Wherein the selection of granularity can prevent coarse whiting raw material surface attachment reaction thing, stops that reaction is carried out; The selection of calcium carbonate slurry concentration had both been beneficial to preparation and conveying, was not easy precipitation and blocking, can not wastes power again, reduce cost.
5, the present invention is preferred, after technique completes one-period, parting liquid in settling tank carries out recycle, and a part is back to reactive crystallization, dense and filtration step as process water and washing water, and another part is for preparing calcium carbonate slurry, migrant worker's industry water can not be re-used like this, turn waste into wealth, reduce environmental protection treatment cost, energy consumption is lower, achieve continuous online recycling spent acid, produce terra alba; And the outer displacement mass after precipitation is stablized, pH value is neutral, and other index all reaches sewage discharge national grade ii standard.
Embodiment
embodiment 1
Utilize aramid II spinning spent acid solution to produce a technique for terra alba, comprise following processing step:
A, spent acid solution pre-treatment
Aramid II spinning spent acid solution is filtered by strainer, then through surge tank, the sulfuric acid concentration fluctuation range in the aramid II spinning spent acid solution described in control;
B, charging
Add in reactive crystallization device by steps A through pretreated aramid II spinning spent acid solution, in reactive crystallization device, add calcium carbonate slurry, the described sulfuric acid in pretreated aramid II spinning spent acid solution and the mol ratio between the calcium carbonate in coarse whiting are 1.02:1 simultaneously;
C, reactive crystallization
The mixing speed controlling reactive crystallization device is 150r/min, and adjusting process water flow velocity is 2m3/h, makes, through pretreated aramid II spinning spent acid solution and calcium carbonate slurry reactive crystallization, to obtain reactive crystallization slurry;
D, dense
The reactive crystallization slurry obtained by step C passes in dense device, carries out solid-liquid separation, improves the mass concentration of terra alba in reactive crystallization slurry;
E, filtration
Reactive crystallization slurry through dense device in step D is passed into vacuum band-type filter machine, filters;
F, precipitation
Slurry through filtering is inputed to settling tank precipitation, solid and liquid separation, the parting liquid obtained and precipitation, precipitation is product terra alba of the present invention.
embodiment 2
Utilize aramid II spinning spent acid solution to produce a technique for terra alba, comprise following processing step:
A, spent acid solution pre-treatment
Aramid II spinning spent acid solution is filtered by strainer, then through surge tank, the sulfuric acid concentration fluctuation range in the aramid II spinning spent acid solution described in control;
B, charging
Add in reactive crystallization device by steps A through pretreated aramid II spinning spent acid solution, in reactive crystallization device, add calcium carbonate slurry, the described sulfuric acid in pretreated aramid II spinning spent acid solution and the mol ratio between the calcium carbonate in coarse whiting are 1.12:1 simultaneously;
C, reactive crystallization
The mixing speed controlling reactive crystallization device is 200r/min, and adjusting process water flow velocity is 6m3/h, makes, through pretreated aramid II spinning spent acid solution and calcium carbonate slurry reactive crystallization, to obtain reactive crystallization slurry;
D, dense
The reactive crystallization slurry obtained by step C passes in dense device, carries out solid-liquid separation, improves the mass concentration of terra alba in reactive crystallization slurry;
E, filtration
Reactive crystallization slurry through dense device in step D is passed into vacuum band-type filter machine, filters;
F, precipitation
Slurry through filtering is inputed to settling tank precipitation, solid and liquid separation, the parting liquid obtained and precipitation, precipitation is product terra alba of the present invention.
embodiment 3
Utilize aramid II spinning spent acid solution to produce a technique for terra alba, comprise following processing step:
A, spent acid solution pre-treatment
Aramid II spinning spent acid solution is filtered by strainer, then through surge tank, the sulfuric acid concentration fluctuation range in the aramid II spinning spent acid solution described in control;
B, charging
Add in reactive crystallization device by steps A through pretreated aramid II spinning spent acid solution, in reactive crystallization device, add calcium carbonate slurry, the described sulfuric acid in pretreated aramid II spinning spent acid solution and the mol ratio between the calcium carbonate in coarse whiting are 1.07:1 simultaneously;
C, reactive crystallization
The mixing speed controlling reactive crystallization device is 175r/min, and adjusting process water flow velocity is 4m3/h, makes, through pretreated aramid II spinning spent acid solution and calcium carbonate slurry reactive crystallization, to obtain reactive crystallization slurry;
D, dense
The reactive crystallization slurry obtained by step C passes in dense device, carries out solid-liquid separation, improves the mass concentration of terra alba in reactive crystallization slurry;
E, filtration
Reactive crystallization slurry through dense device in step D is passed into vacuum band-type filter machine, filters;
F, precipitation
Slurry through filtering is inputed to settling tank precipitation, solid and liquid separation, the parting liquid obtained and precipitation, precipitation is product terra alba of the present invention.
embodiment 4
Utilize aramid II spinning spent acid solution to produce a technique for terra alba, comprise following processing step:
A, spent acid solution pre-treatment
Aramid II spinning spent acid solution is filtered by strainer, then through surge tank, the sulfuric acid concentration fluctuation range in the aramid II spinning spent acid solution described in control;
B, charging
Add in reactive crystallization device by steps A through pretreated aramid II spinning spent acid solution, in reactive crystallization device, add calcium carbonate slurry, the described sulfuric acid in pretreated aramid II spinning spent acid solution and the mol ratio between the calcium carbonate in coarse whiting are 1.1:1 simultaneously;
C, reactive crystallization
The mixing speed controlling reactive crystallization device is 186r/min, and adjusting process water flow velocity is 5m3/h, makes, through pretreated aramid II spinning spent acid solution and calcium carbonate slurry reactive crystallization, to obtain reactive crystallization slurry;
D, dense
The reactive crystallization slurry obtained by step C passes in dense device, carries out solid-liquid separation, improves the mass concentration of terra alba in reactive crystallization slurry;
E, filtration
Reactive crystallization slurry through dense device in step D is passed into vacuum band-type filter machine, filters;
F, precipitation
Slurry through filtering is inputed to settling tank precipitation, solid and liquid separation, the parting liquid obtained and precipitation, precipitation is product terra alba of the present invention.
embodiment 5
On the basis of embodiment 1-4, preferred:
In step, the precision of described strainer is 150 orders.
In step, the volume of described surge tank is 8 times of described aramid II spinning spent acid solution generation volume per hour.
In stepb, the coarse whiting mass percent in described calcium carbonate slurry is 8%, and wherein coarse whiting granularity is 150 orders, CaCO
3content is 95%, and whiteness is 93%.
In step D, in described raising reactive crystallization slurry, the mass concentration of terra alba refers to and the mass concentration of terra alba in reactive crystallization slurry is brought up to 35%.
In step e, the vacuum degree control of described vacuum band-type filter machine is-0.06MPa, and the water content control through the reactive crystallization slurry of vacuum band-type filter machine filtration is 5%, and whiteness is 85%.
embodiment 6
On the basis of embodiment 1-4, preferred:
In step, the precision of described strainer is 250 orders.
In step, the volume of described surge tank is 12 times of described aramid II spinning spent acid solution generation volume per hour.
In stepb, the coarse whiting mass percent in described calcium carbonate slurry is 10%, and wherein coarse whiting granularity is 200 orders, CaCO
3content is 99%, and whiteness is 98%.
In step D, in described raising reactive crystallization slurry, the mass concentration of terra alba refers to and the mass concentration of terra alba in reactive crystallization slurry is brought up to 45%.
In step e, the vacuum degree control of described vacuum band-type filter machine is-0.08MPa, and the water content control through the reactive crystallization slurry of vacuum band-type filter machine filtration is 22%, and whiteness is 95%.
embodiment 7
On the basis of embodiment 1-4, preferred:
In step, the precision of described strainer is 200 orders.
In step, the volume of described surge tank is 10 times of described aramid II spinning spent acid solution generation volume per hour.
In stepb, the coarse whiting mass percent in described calcium carbonate slurry is 9%, and wherein coarse whiting granularity is 175 orders, CaCO
3content is 97%, and whiteness is 95.5%.
In step D, in described raising reactive crystallization slurry, the mass concentration of terra alba refers to and the mass concentration of terra alba in reactive crystallization slurry is brought up to 40%.
In step e, the vacuum degree control of described vacuum band-type filter machine is-0.07MPa, and the water content control through the reactive crystallization slurry of vacuum band-type filter machine filtration is 13.5%, and whiteness is 90%.
embodiment 8
On the basis of embodiment 1-4, preferred:
In step, the precision of described strainer is 210 orders.
In step, the volume of described surge tank is 9.5 times of described aramid II spinning spent acid solution generation volume per hour.
In stepb, the coarse whiting mass percent in described calcium carbonate slurry is 8.5%, and wherein coarse whiting granularity is 165 orders, CaCO
3content is 98%, and whiteness is 96%.
In step D, in described raising reactive crystallization slurry, the mass concentration of terra alba refers to and the mass concentration of terra alba in reactive crystallization slurry is brought up to 42%.
In step e, the vacuum degree control of described vacuum band-type filter machine is-0.075MPa, and the water content control through the reactive crystallization slurry of vacuum band-type filter machine filtration is 17%, and whiteness is 88%.
embodiment 9
On the basis of embodiment 1-8, preferred:
The described aramid II spinning spent acid solution that utilizes is produced in the technique one-period of terra alba, after step F obtains terra alba by precipitation, the parting liquid part reuse obtained is to reactive crystallization, dense and filtration step, and another part is for preparing calcium carbonate slurry.
Described settling tank and described reactive crystallization device, by two communication, form inner cycle channel.
Process water overflow in described dense device is to vacuum band-type filter machine and settling tank.
In the method for above-mentioned utilization process water:
Under to meet process water flow velocity in reactive crystallization step be the condition of 2 ~ 6m3/h, reactive crystallization device is 9 ~ 13m3/h by pipeline to the flow velocity of settling tank overflow; Meanwhile, dense device is all 2 ~ 3m3/h to the spillway discharge of vacuum band-type filter machine and settling tank.
Claims (6)
1. utilize aramid II spinning spent acid solution to produce a technique for terra alba, it is characterized in that: comprise following processing step:
A, spent acid solution pre-treatment
Aramid II spinning spent acid solution is filtered by strainer, then through surge tank, the sulfuric acid concentration fluctuation range in the aramid II spinning spent acid solution described in control; The precision of described strainer is 150 ~ 250 orders; The volume of described surge tank is 8 ~ 12 times of described aramid II spinning spent acid solution generation volume per hour;
B, charging
Add in reactive crystallization device by steps A through pretreated aramid II spinning spent acid solution, in reactive crystallization device, add calcium carbonate slurry, the described sulfuric acid in pretreated aramid II spinning spent acid solution and the mol ratio between the calcium carbonate in coarse whiting are 1.02 ~ 1.12:1 simultaneously; Coarse whiting mass percent in described calcium carbonate slurry is 8 ~ 10%, and wherein coarse whiting granularity is 150 ~ 200 orders, CaCO
3content>=95%, whiteness>=93%;
C, reactive crystallization
The mixing speed controlling reactive crystallization device is 150 ~ 200r/min, and adjusting process water flow velocity is 2 ~ 6m3/h, makes, through pretreated aramid II spinning spent acid solution and calcium carbonate slurry reactive crystallization, to obtain reactive crystallization slurry; In described reactive crystallization device, pH is 6 ~ 8;
D, dense
The reactive crystallization slurry obtained by step C passes in dense device, carries out solid-liquid separation, improves the mass concentration of terra alba in reactive crystallization slurry;
E, filtration
Reactive crystallization slurry through dense device in step D is passed into vacuum band-type filter machine, filters;
F, precipitation
Slurry through filtering is inputed to settling tank precipitation, solid and liquid separation, the parting liquid obtained and precipitation, precipitation is terra alba.
2. a kind of technique utilizing aramid II spinning spent acid solution to produce terra alba according to claim 1, it is characterized in that: in step D, in described raising reactive crystallization slurry, the mass concentration of terra alba refers to and the mass concentration of terra alba in reactive crystallization slurry is brought up to 35 ~ 45%.
3. a kind of technique utilizing aramid II spinning spent acid solution to produce terra alba according to claim 1, it is characterized in that: in step e, the vacuum degree control of described vacuum band-type filter machine is-0.06 ~-0.08MPa, water content control through the reactive crystallization slurry of vacuum band-type filter machine filtration is≤22%, whiteness >=85%.
4. a kind of technique utilizing aramid II spinning spent acid solution to produce terra alba according to claim 1, it is characterized in that: the described aramid II spinning spent acid solution that utilizes is produced in the technique one-period of terra alba, after step F obtains terra alba by precipitation, the parting liquid part reuse obtained is to reactive crystallization, dense and filtration step, and another part is for preparing calcium carbonate slurry.
5. a kind of technique utilizing aramid II spinning spent acid solution to produce terra alba according to claim 4, is characterized in that: described settling tank and described reactive crystallization device, by two communication, form inner cycle channel.
6. a kind of technique utilizing aramid II spinning spent acid solution to produce terra alba according to claim 4 or 5, is characterized in that: the process water overflow in described dense device is to vacuum band-type filter machine and settling tank.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103693670B (en) * | 2013-12-16 | 2015-07-22 | 乳源瑶族自治县东阳光化成箔有限公司 | Production method of calcium sulphate dehydrate and production device thereof |
| CN104016398B (en) * | 2014-06-23 | 2016-07-06 | 武善东 | A kind of method that dilute sulfuric acid utilized in industrial wastewater produces sulfate |
| CN109502625A (en) * | 2018-12-26 | 2019-03-22 | 蓝星（成都）新材料有限公司 | The technique that gypsum is prepared using acid pickle |
| CN111018382A (en) * | 2019-12-30 | 2020-04-17 | 中芳特纤股份有限公司 | Method for preparing high-strength gypsum by using para-aramid spinning waste acid and waste silk |
| CN111484062A (en) * | 2020-04-15 | 2020-08-04 | 江苏一夫科技股份有限公司 | Calcium sulfate dihydrate, preparation method and application thereof |
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