CN1341558A - Method for preparing potassium sulfate - Google Patents

Abstract

The improved preparation method of potassium sulfate includes the following steps: 1. preparing raw materials, 2. filter pressing; 3. association; 4. separation; 5. adding (45%-55% of) demulsifying agent in the residual solution after the solid potassium sulfate is separated out, the demulsifying agent is one of the following materials; benzenesulfonic acid, sodium benzenesulfonate, butylsulfonic acid, sodium butylsulfonate, oxalic acid, sodium oxalate, citric acid, sodium citrate, salicylic acid, sodium salicylate, 5-sulfosalicylic acid, 8-hydroxyquinoline and 2-methyl-8-hydroxyquinoline, and the total added quantity of demulsifying agent is 1.5-300 times of impurity weight contained in the raw material; 6. preparing regeneration solution; 7. deassociation; and 8. adding the residual demulsifying agent into residual ammonium chloride mother liquor after the solid ammonium chloride is separated out as regeneration solution and can be reused. It can retain activity of association agent and can ensure normal production.

Description

A kind of method for preparing vitriolate of tartar

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, obtain solution, the container of packing into according to predetermined ratio;

(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 preset temperature, to form and put agent and squeeze into heat exchanger heats to preset temperature, 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 preset temperature, 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 1.5～300 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 an amount of free ammonia with the mother liquor that contains an amount of concentration ammonium chloride by absorbing gas ammonia;

(7) separate and form, to form the oil phase thing of putting the reaction generation with pump and squeeze into heater heats to preset temperature, 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 to certain temperature, become the ammonium chloride finished product through the evaporation concentration postcooling;

(9) add emulsion splitter, the emulsion splitter of remaining (55%～45%) is joined separate out behind the chloride solid in the remaining ammonium chloride mother liquor, return regeneration container configuration regenerated liquid and reuse.

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.

The specific embodiment: the present invention is described in further details below in conjunction with accompanying drawing. Of the present inventionization Learn reaction principle and main production flow process and " a kind of method of preparing potassium sulfate " (patent No. 88105025.3) patented technology identical. Main feature of the present invention is the problem that solves above-mentioned patented technology, Namely cause forming the active problem that constantly descends of putting agent owing to containing inevitably impurity in the raw material. By Can put the agent effect and generate emulsion with forming in impurity, make to form and put the agent loss of activity, therefore, deal with problems Key is prevention impurity and forms and put agent effect generation emulsion. Used demulsifier can be following material it One: benzene sulfonic acid, benzene sulfonic acid sodium salt, fourth sulfonic acid, fourth sodium sulfonate, oxalic acid, sodium oxalate, citric acid, lemon Acid sodium, salicylic acid, sodium salicylate, 5-sulfo group-salicylic acid, oxine, 2-methyl-8-hydroxyl quinoline Quinoline. Total addition of demulsifier is 1.5～300 times of impurities weight in the raw material. The content of impurity can To obtain by chemically examining to the chemical examination of raw material with to the tracking of solution in the production process. The adding branch of demulsifier Being twice, once is after isolating the potassium sulfate solid, will separate out after the solid sulphuric acid potassium remaining molten Liquid is extracted in the container, adds the demulsifier that accounts for total amount (45%～55%) in solution, generally can Add 50%. The solution that is added with demulsifier will be sent in the proportion container as raw material and reuse. Another time is After isolating chloride solid, the demulsifier of remaining (55%～45%) joined separate out chlorination In the remaining ammonium chloride mother liquor, return regeneration container configuration regenerated liquid and reuse behind the ammonium solid.

Embodiment.

The raw material proportioning of producing potassium sulfate is:

Sulfuric acid: 1～15%

Potassium chloride: 7～27%

Form and put agent: 25～50%

Potassium sulfate: 3～20%

Regenerated liquid: ammonium chloride solution, free ammonia wherein are 3～14%

Ammonium chloride: 5～35%

Water: surplus

Demulsifier: 1.5～300 times of content of impurities.

Because the basic process of production and " a kind of method of preparing potassium sulfate " (patent No. 88105025.3) Patent is identical, is not repeating at this. Mainly the composition of the demulsifier of twice adding and total quantity row Go out. When total weight of material of chemical reaction is 30 tons, according to chemical examination, when impurity content was 0.2%, institute added The demulsifier that enters is any one in the following material, auspiciously sees Table 1.

The weight of the total material of table 1 reaction is 30 tons, demulsifier scale during impurity content 0.2%

Sequence number	Demulsifier	Gross weight Kg	Addition Kg for the first time	The demulsifier total amount is the multiple of impurity
					Embodiment 1	Benzene sulfonic acid	150	75	10
Embodiment 2	Benzene sulfonic acid sodium salt	168	84	12
					Embodiment 3	Fourth sulfonic acid	300	135	20
Embodiment 4	The fourth sodium sulfonate	332	176	23
					Embodiment 5	Oxalic acid	450	225	30
Embodiment 6	Sodium oxalate	463	236	37
					Embodiment 7	Citric acid	410	200	27
Embodiment 8	Natrium citricum	423	212	28
					Embodiment 9	Salicylic acid	195	98	13
Embodiment 10	Sodium salicylate	213	110	15

Embodiment 11	5-sulfo group-salicylic acid	247	135	16
					Embodiment 12	Oxine	630	315	42
Embodiment 13	2-methyl-oxine	750	360	50

Stirred 30 minutes after adding demulsifier, leave standstill and to use in 3 hours. Through actual measurement, form the work of putting agent Property does not reduce.

When total weight of material of chemical reaction is 30 tons, according to chemical examination, when impurity content is 0.15%, institute The demulsifier that adds is any one in the following material, auspiciously sees Table 2.

The weight of the total material of table 2 reaction is 30 tons, demulsifier scale during impurity content 0.15%

Sequence number	Demulsifier	Gross weight Kg	Addition Kg for the first time	The demulsifier total amount is the multiple of impurity
					Embodiment 15	Benzene sulfonic acid	450	225	30
Embodiment 16	Benzene sulfonic acid sodium salt	504	252	33
					Embodiment 17	Fourth sulfonic acid	675	305	45
Embodiment 18	The fourth sodium sulfonate	747	358	50
					Embodiment 19	Oxalic acid	900	495	60
Embodiment 20	Sodium oxalate	926	481	62
					Embodiment 21	Citric acid	1200	600	80
Embodiment 22	Natrium citricum	1250	625	83
					Embodiment 23	Salicylic acid	580	290	38
Embodiment 24	Sodium salicylate	594	297	40
					Embodiment 25	5-sulfo group-salicylic acid	675	340	45
Embodiment 26	Oxine	694	330	47
					Embodiment 27	2-methyl-oxine	757	380	50

Add demulsifier by actual measurement, form the activity of putting agent and do not reduce.

Claims (1)

1, a kind of method for preparing vitriolate of tartar is characterized in that,

(1) batching takes by weighing various raw materials, obtain solution, the container of packing into according to predetermined ratio;

(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 preset temperature, to form and put agent and squeeze into heat exchanger heats to preset temperature, 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 preset temperature, 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 1.5～300 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 an amount of free ammonia with the mother liquor that contains an amount of concentration ammonium chloride by absorbing gas ammonia;

(7) separate and form, to form the oil phase thing of putting the reaction generation with pump and squeeze into heater heats to preset temperature, 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 to certain temperature, become the ammonium chloride finished product through the evaporation concentration postcooling;

(9) add emulsion splitter, the emulsion splitter of remaining (55%～45%) is joined separate out behind the chloride solid in the remaining ammonium chloride mother liquor, return regeneration container configuration regenerated liquid and reuse.