CN1164492C - Method for preparing potassium sulfate - Google Patents
Method for preparing potassium sulfate Download PDFInfo
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- CN1164492C CN1164492C CNB011419695A CN01141969A CN1164492C CN 1164492 C CN1164492 C CN 1164492C CN B011419695 A CNB011419695 A CN B011419695A CN 01141969 A CN01141969 A CN 01141969A CN 1164492 C CN1164492 C CN 1164492C
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Abstract
The present invention relates to an improvement to a preparation method which belongs to the field of chemical technology. The method of the present invention has the technological steps: 1. material preparation is carried out; 2. filter pressing is carried out; 3. association displacement is carried out 4. separation is carried out; 5.45% to 55% of demulsifying agents are added in residual solution after solid potassium sulfate is separated out; 6. actified solution is prepared; 7. association release is carried out; 8. the residual demulsifying agents are added in residual ammonium chloride mother solution in which solid ammonium chloride is separated out to be used as actified solution to be reused. The demulsifying agents are one of benzenesulfonic acid, sodium benzenesulfonate, butylsulfonic acid, sodium butylsulfonate, oxalic acid, sodium oxalate, citric acid, sodium citrate, salicylic acid, sodium salicylate, 5-sulfo-salicylic acid, 8-hydroxyquinoline and 2-methyl-8-hydroxyquinoline. the weight of all the added demulsifying agents are 1.5 to 300 times than the weight of impurities contained in raw materials; the present invention can keep the activity of association displacement agents and enables the production to be in normal operation.
Description
Technical field: the invention belongs to chemical technology field, relate to improvement to the vitriolate of tartar preparation method.
Background technology: the name of Shenyang Institute of Chemical Comprehensive Utilization is called in the patent documentation of " a kind of method of producing vitriolate of tartar " (patent No. 88105025.3), discloses a kind of preparation method of vitriolate of tartar.This method is used raw materials such as sulfuric acid, Repone K, vitriolate of tartar, ammonium chloride, ammonia, water, do to form with the mixture of trialkyl tertiary amine and thinner and put agent, put reaction and generate vitriolate of tartar by forming, form reaction and generate byproduct ammonium chloride, form and put agent and can reuse by separating.This method compared with additive method technology simple, utilize " three wastes ", low cost and other advantages.But,, find that there is the problem of forming activity continuous decline owing to the continuous introducing of impurity of putting agent in this method through the practice of suitability for industrialized production, cause forming and put the agent extraction ability and constantly descend, make and form the consumption of putting agent and constantly increase, product cost raises, and finally causes producing carrying out.
Summary of the invention: technical problem to be solved by this invention is, provide a kind of based on aforementioned production method, can overcome because of impurity causes and form the vitriolate of tartar preparation method who puts the agent degradation, form the activity of putting agent to remain, keep the normal operation of production process.
Technical scheme of the present invention is, a kind of method for preparing vitriolate of tartar is characterized in that,
(1) batching takes by weighing various raw materials according to following ratio, obtain solution, and the container of packing into:
Sulfuric acid: 1～15%
Repone K: 7～27%
Form and put agent: 25～50%
Vitriolate of tartar: 3～20%
Regenerated liquid: ammonium chloride solution, free ammonia wherein are 3～14%
Ammonium chloride: 5～35%
Water: surplus;
(2) press filtration is squeezed into pressure filter with material solution by pump, and insolubles is filtered out;
(3) form and put, by pump material solution is squeezed into heat exchanger heats to 5～150 ℃, to form and put agent and squeeze into heat exchanger heats to 5～150 ℃, then above-mentioned two kinds of materials are squeezed into to form to put to form in the reactor and put reaction, the solution layering of reaction back, the upper strata is the oil phase thing, and lower floor is the solidliquid mixture of vitriolate of tartar and Repone K;
(4) separate, the vitriolate of tartar of solution lower floor and the solidliquid mixture of Repone K are extracted out, be cooled to 10 ℃, solid sulphuric acid potassium is separated out, put into whizzer, become the finished product vitriolate of tartar solid sulphuric acid potassium and liquid separation;
(5) add emulsion splitter, rest solution is extracted in the container after will separating out solid sulphuric acid potassium, in solution, add the emulsion splitter that accounts for total amount 45%～55%, emulsion splitter is one of following material: Phenylsulfonic acid, benzene sulfonic acid sodium salt, fourth sulfonic acid, fourth sodium sulfonate, oxalic acid, sodium oxalate, citric acid, Trisodium Citrate, Whitfield's ointment, sodium salicylate, 5-sulfo group-Whitfield's ointment, oxine, 2-methyl-oxine, total add-on of emulsion splitter are 1.5～27.8 times of impurities weight in the raw material; The solution that is added with emulsion splitter is sent in the proportion container as raw material and is reused;
(6) regenerated liquid preparation becomes the regenerated liquid that contains free ammonia 3～14% with the mother liquor that contains chlorination ammonium concentration 5～35% by absorbing gas ammonia;
(7) separate and form, to form with pump and to put oil phase thing that reaction produces and squeeze into heater heats to 5～150 ℃, squeeze into then to separate and form reactor, simultaneously regenerated liquid is also squeezed into to separate and form reactor, form reaction separating to form to separate in the reactor, the reaction back generates two layers of solution, and the upper strata is formed for the oil phase thing and put agent, lower floor is an ammonium chloride solution
(8) separate, from separate lower floor's solution of forming reactor, extract ammonium chloride solution out, ℃ separate out chloride solid, become the ammonium chloride finished product through evaporation concentration postcooling to 10～20;
(9) add emulsion splitter, the emulsion splitter with remaining 55%～45% joins separates out behind the chloride solid in the remaining ammonium chloride mother liquor, returns regeneration container configuration regenerated liquid and reuses.
The invention has the beneficial effects as follows, put at causing because of the impurity that is contained in the raw material to form that the agent extraction ability descends, the active phenomenon that reduces, take to add the influence that emulsion splitter is eliminated impurity, stop impurity to put the agent effect and generate emulsification with forming, kept forming the activity of putting agent, production is normally carried out.Test shows, method of the present invention is compared with the patented technology actual motion effect of above-mentioned existing " a kind of method of producing vitriolate of tartar " (patent No. 88105025.3), form the consumption of putting agent and reduced more than 50%, the economic benefit of producing vitriolate of tartar per ton has improved 300 yuan.
Description of drawings: Fig. 1 is a Production Flow Chart synoptic diagram of the present invention.Among the figure, 1 is burden process, and 2 for press filtration, and 3 put for forming, and 4 for separating the finished product vitriolate of tartar, and 5 for adding emulsion splitter, and 6 are the regenerated liquid preparation, and 7 form for separating, and 8 is separation byproduct ammonium chloride, and 9 is to add emulsion splitter the second time.
Embodiment: the present invention is described in further details below in conjunction with accompanying drawing.Chemical principle of the present invention is identical with the patented technology of " a kind of method of producing vitriolate of tartar " (patent No. 88105025.3) with the main production flow process.Principal feature of the present invention is the problem that solves above-mentioned patented technology, promptly causes forming the active problem that constantly descends of putting agent owing to containing impurity in the raw material inevitably.Because impurity can be put the agent effect and generate emulsification with forming, make to form and put the agent loss of activity, therefore, the key of dealing with problems is to stop impurity to put the agent effect and generate emulsification with forming.Used emulsion splitter can be one of following material: Phenylsulfonic acid, benzene sulfonic acid sodium salt, fourth sulfonic acid, fourth sodium sulfonate, oxalic acid, sodium oxalate, citric acid, Trisodium Citrate, Whitfield's ointment, sodium salicylate, 5-sulfo group-Whitfield's ointment, oxine, 2-methyl-oxine.Total add-on of emulsion splitter is 1.5～27.8 times of impurities weight in the raw material.The content of impurity can obtain by chemically examining to the chemical examination of raw material with to the tracking of solution in the production process.The adding of emulsion splitter is divided into twice, once is after isolating the vitriolate of tartar solid, will separate out the later rest solution of solid sulphuric acid potassium and be extracted in the container, adds the emulsion splitter that accounts for total amount 45%～55% in solution, generally can add 50%.The solution that is added with emulsion splitter will be sent in the proportion container as raw material and reuse.Another time is after isolating chloride solid, and the emulsion splitter with remaining 55%～45% joins separates out behind the chloride solid in the remaining ammonium chloride mother liquor, returns regeneration container configuration regenerated liquid and reuses.
Embodiment.
The proportioning raw materials of producing vitriolate of tartar is:
Sulfuric acid: 1～15%
Repone K: 7～27%
Form and put agent: 25～50%
Vitriolate of tartar: 3～20%
Regenerated liquid: ammonium chloride solution, free ammonia wherein are 3～14%
Ammonium chloride: 5～35%
Water: surplus
Emulsion splitter: 1.5～27.8 times of content of impurities.
Because the basic process of production is identical with the patent of " a kind of method of producing vitriolate of tartar " (patent No. 88105025.3), do not repeating at this.Mainly the composition of the emulsion splitter of twice adding and total quantity are listed.When total weight of material of chemical reaction is 30 tons, according to chemical examination, foreign matter content is 0.2% o'clock, and the emulsion splitter that is added is any one in the following material, auspiciously sees Table 1.
The weight of the total material of table 1 reaction is 30 tons, emulsion splitter scale during foreign matter content 0.2%
| Sequence number | Emulsion splitter | Gross weight Kg | Add-on Kg for the first time | The emulsion splitter total amount is the multiple of |
| Embodiment | ||||
| 1 | Phenylsulfonic acid | 150 | 75 | 2.5 |
| | Benzene sulfonic acid sodium salt | 168 | 84 | 2.8 |
| | Fourth sulfonic acid | 300 | 135 | 5.0 |
| Embodiment 4 | The fourth sodium sulfonate | 332 | 176 | 5.5 |
| | Oxalic acid | 450 | 225 | 7.5 |
| | Sodium oxalate | 463 | 236 | 7.7 |
| | Citric acid | 410 | 200 | 6.8 |
| | Trisodium Citrate | 423 | 212 | 7.1 |
| | Whitfield's ointment | 195 | 98 | 3.3 |
| Embodiment 10 | Sodium salicylate | 213 | 110 | 3.6 |
| Embodiment 11 | 5-sulfo group-Whitfield's ointment | 247 | 135 | 4.1 |
| Embodiment 12 | Oxine | 630 | 315 | 10.5 |
| Embodiment 13 | 2-methyl-oxine | 750 | 360 | 12.5 |
Stirred 30 minutes after adding emulsion splitter, leave standstill and to use in 3 hours.Through actual measurement, form the activity of putting agent and do not reduce.
When total weight of material of chemical reaction is 30 tons, according to chemical examination, foreign matter content is 0.15% o'clock, and the emulsion splitter that is added is any one in the following material, auspiciously sees Table 2.
The weight of the total material of table 2 reaction is 30 tons, emulsion splitter scale during foreign matter content 0.15%
| Sequence number | Emulsion splitter | Gross weight Kg | Add-on Kg for the first time | The emulsion splitter total amount is the multiple of impurity |
| Embodiment 15 | Phenylsulfonic acid | 450 | 225 | 10 |
| Embodiment 16 | Benzene sulfonic acid sodium salt | 504 | 252 | 11.2 |
| Embodiment 17 | Fourth sulfonic acid | 675 | 305 | 15 |
| Embodiment 18 | The fourth sodium sulfonate | 747 | 358 | 16.6 |
| Embodiment 19 | Oxalic acid | 900 | 495 | 20 |
| Embodiment 20 | Sodium oxalate | 926 | 481 | 20.6 |
| Embodiment 21 | Citric acid | 1200 | 600 | 26.7 |
| Embodiment 22 | Trisodium Citrate | 1250 | 625 | 27.8 |
| Embodiment 23 | Whitfield's ointment | 580 | 290 | 12.9 |
| Embodiment 24 | Sodium salicylate | 594 | 297 | 13.2 |
| Embodiment 25 | 5-sulfo group-Whitfield's ointment | 675 | 340 | 15 |
| Embodiment 26 | Oxine | 694 | 330 | 15.4 |
| Embodiment 27 | 2-methyl-oxine | 757 | 380 | 16.8 |
Add emulsion splitter after actual measurement is formed the activity of putting agent and do not reduced.
Claims (1)
1, a kind of method for preparing vitriolate of tartar is characterized in that,
(1) batching takes by weighing various raw materials according to following ratio, obtain solution, and the container of packing into:
Sulfuric acid: 1～15%
Repone K: 7～27%
Form and put agent: 25～50%
Vitriolate of tartar: 3～20%
Regenerated liquid: ammonium chloride solution, free ammonia wherein are 3～14%
Ammonium chloride: 5～35%
Water: surplus;
(2) press filtration is squeezed into pressure filter with material solution by pump, and insolubles is filtered out;
(3) form and put, by pump material solution is squeezed into heat exchanger heats to 5～150 ℃, to form and put agent and squeeze into heat exchanger heats to 5～150 ℃, then above-mentioned two kinds of materials are squeezed into to form to put to form in the reactor and put reaction, the solution layering of reaction back, the upper strata is the oil phase thing, and lower floor is the solidliquid mixture of vitriolate of tartar and Repone K;
(4) separate, the vitriolate of tartar of solution lower floor and the solidliquid mixture of Repone K are extracted out, be cooled to 10 ℃, solid sulphuric acid potassium is separated out, put into whizzer, become the finished product vitriolate of tartar solid sulphuric acid potassium and liquid separation;
(5) add emulsion splitter, rest solution is extracted in the container after will separating out solid sulphuric acid potassium, in solution, add the emulsion splitter that accounts for total amount 45%～55%, emulsion splitter is one of following material: Phenylsulfonic acid, benzene sulfonic acid sodium salt, fourth sulfonic acid, fourth sodium sulfonate, oxalic acid, sodium oxalate, citric acid, Trisodium Citrate, Whitfield's ointment, sodium salicylate, 5-sulfo group-Whitfield's ointment, oxine, 2-methyl-oxine, total add-on of emulsion splitter are 1.5～27.8 times of impurities weight in the raw material; The solution that is added with emulsion splitter is sent in the proportion container as raw material and is reused;
(6) regenerated liquid preparation becomes the regenerated liquid that contains free ammonia 3～14% with the mother liquor that contains chlorination ammonium concentration 5～35% by absorbing gas ammonia;
(7) separate and form, to form with pump and to put oil phase thing that reaction produces and squeeze into heater heats to 5～150 ℃, squeeze into then to separate and form reactor, simultaneously regenerated liquid is also squeezed into to separate and form reactor, form reaction separating to form to separate in the reactor, the reaction back generates two layers of solution, and the upper strata is formed for the oil phase thing and put agent, lower floor is an ammonium chloride solution
(8) separate, from separate lower floor's solution of forming reactor, extract ammonium chloride solution out, ℃ separate out chloride solid, become the ammonium chloride finished product through evaporation concentration postcooling to 10～20;
(9) add emulsion splitter, the emulsion splitter with remaining 55%～45% joins separates out behind the chloride solid in the remaining ammonium chloride mother liquor, returns regeneration container configuration regenerated liquid and reuses.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011419695A CN1164492C (en) | 2001-09-26 | 2001-09-26 | Method for preparing potassium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011419695A CN1164492C (en) | 2001-09-26 | 2001-09-26 | Method for preparing potassium sulfate |
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| Publication Number | Publication Date |
|---|---|
| CN1341558A CN1341558A (en) | 2002-03-27 |
| CN1164492C true CN1164492C (en) | 2004-09-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011419695A Expired - Fee Related CN1164492C (en) | 2001-09-26 | 2001-09-26 | Method for preparing potassium sulfate |
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| CN114590820A (en) * | 2022-03-10 | 2022-06-07 | 四川西陇科学有限公司 | Purification method of potassium-containing ammonium chloride |
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