CN1044111C

CN1044111C - Potash and nitrogenous fertilizer mfg. process from illite

Info

Publication number: CN1044111C
Application number: CN92105286A
Authority: CN
Inventors: 冯振普; 韩佩志; 范富荣
Original assignee: Individual
Current assignee: Individual
Priority date: 1992-07-01
Filing date: 1992-07-01
Publication date: 1999-07-14
Anticipated expiration: 2007-07-01
Also published as: CN1066645A

Abstract

The present invention relates to a method for preparing potash fertilizer from ore. The present invention takes illite as a raw material and adopts sulphuric acid for low-temperature decomposition, and meanwhile, byproducts of active silicon dioxide, aluminum sulfate and aluminum hydroxide can be produced. The potassium extracting rate of the present invention is 90%, the crude ore utilizing rate is approximate to 100%, and each ton of illite can produce 650kg of potassic and nitrogenous fertilizer, wherein the content of K2O is not smaller than 11%, and the content of N is not smaller than 15%. Compared with a high-temperature roasting method of a traditional kiln, the present invention has the advantages of good energy-saving effect, less investment, obvious effect, simple technology, easy operation, no gangue, no pollution and good comprehensive utilization effect; a new resource is inaugurated for the industrial production of potassic fertilizer, and meanwhile, the present invention also belongs to further increment exploitation for illite.

Description

Produce the method for potassium-nitrogen fertilizer with illite

The present invention relates to a kind ofly produce the method for potash fertilizer, particularly produce potassium-nitrogen fertilizer, simultaneously the method for output active silica, Tai-Ace S 150 and aluminium hydroxide byproduct with the sulfuric acid to leach illite with the ore deposit rock.The present invention is to illitic further increment exploitation.

Potash fertilizer is one of a large amount of three big chemical fertilizer that use in the agricultural, and plant-growth is essential.Potash fertilizer kind relatively tube is single, and about 95% is Repone K, and sulfate type potash fertilizer accounts for 5%, also has nitric acid, carbonic acid and the phosphoric acid salt potash fertilizer of minute quantity.The raw material of potash fertilizer industry mainly is the soluble potassium salt mine at present, wherein sylvite and mixing salt thereof occupy the position of particularly important in potash fertilizer production, the potash fertilizer factory of world's overall throughput 96% in 1985 makes raw material with it, also has other raw material such as the face of land or subsurface brine etc. in addition.The potash fertilizer production of China is comparatively backward, and the raw material that is adopted has bittern, alunite or other rich potassic rock etc., and production technique mostly is the energy consumption height, investment is big, chemical pollution is serious, the High-temp. kiln roasting method of comprehensive utilization weak effect.Because raw material resources poorness, add that production technique falls behind, the present potash fertilizer output of China only is 2% of demand, 98% need be from external import, this is serious problem beyond doubt the salty many China of owner with the agricultural concerning one, particularly current people are the economical farm crop of emphasis on development more, and growing to sulfate type potash fertilizer demand, disparities between supply and demand day is becoming tight.In order to alleviate this pressure, people are striving to find always and can develop the new resources of producing potash fertilizer.We find through tests up to a hundred time, and the illite of very easily exploiting in the many areas of China not only can be used for producing potash fertilizer, and also has high comprehensive utilization value.And before this, illite just is used for doing papermaking filler, or plastics, loading material of rubber and ceramic raw material etc., fails well to be developed.Through retrieving about the patent documentation of producing potash fertilizer with the ore deposit rock domestic and international, not having to find with the illite is the potash fertilizer industry production of raw material.

Purpose of the present invention is intended to produce china natural resources poorness particularly, raw material variety is few, production technique falls behind present situation at current potash fertilizer industry, a kind of method of producing vitriolate of tartar nitrogenous fertilizer with new mineral wealth and new technology is proposed, to enlarge the raw material variety of potash fertilizer industry, improve the turnout of sulfate type potash fertilizer, overcome defectives such as investment is big in the existing technology, energy consumption is high, seriously polluted, comprehensive utilization weak effect, to satisfy the heavy demand of current China, also be simultaneously to propose a kind of further exploitation illite to make its value-added new way to potash fertilizer.

For achieving the above object, the technical solution of the present invention's proposition is: with illite (K, H ₂O) Al ₂[AlSi ₃O ₁₀] (H ₂O, OH) ₂Be raw material, it is pulverized the back drops in the reactor, the sulfuric acid of adding 50～60%, the sulfuric acid add-on is: 92% sulfuric acid: powder=1: 1, react 135～145 ℃ of temperature of reaction under agitation condition, reaction pressure 0.3～0.4Mpa, 175～185 minutes reaction times, react to pH value be 1～2 o'clock, add Al ₂O ₃Transferring pH value is that 3 afterreactions finish, add hot water dilution after-filtration, filter residue is active silica after cleaning, filtrate is separated after inspissation, crystallization, and the surplus liquid of crystallization is produced Tai-Ace S 150 through further inspissation crystallization inspissation, adds the water heating with still during crystalline solid is moved into and makes it become solution, add the bicarbonate of ammonia neutralization then, reacting to pH value is to finish in 6.5～7 o'clock, and the filter residue after the filtration is aluminium hydroxide through washing, and potassium-nitrogen fertilizer is produced in the concentrating filter liquor crystallization.

Accompanying drawing is depicted as the technical process schematic block diagram of producing vitriolate of tartar nitrogenous fertilizer with illite.

Below with reference to Figure of description and embodiment the present invention is done further detailed description, among the figure 1: pulverize; 2: sulfuric acid reaction; 3: filter; 4: washing; 5: mix; 6: the inspissation crystallization; 7: separate; 8: the inspissation crystallization; 9: be dissolved in water; 10: neutralization; 11: filtering separation; 12: washing; 13: mix; 14: condensing crystal.

As shown in drawings, with illite (K, H ₂O) Al ₂[AlSi ₃O ₁₀] (H ₂O, OH) ₂For raw material it is pulverized 1, make powder A; Raw ore is pulverized fineness requirement 110～120 orders through jaw crusher, Raymond mill two-stage.Powder A is dropped in the reactor, add 50～60% sulfuric acid, the sulfuric acid add-on is: 92% sulfuric acid: powder A=1: 1, under agitation condition, react 2,135～145 ℃ of temperature of reaction, reaction pressure 0.3～0.4Mpa, 175～185 minutes reaction times, react to pH value be 1～2 o'clock, add Al ₂O ₃Transferring pH value is that 3 afterreactions 2 finish.Reaction 2 has solid precipitation B to generate, and reaction solution C is the mixed solution of Tai-Ace S 150 and vitriolate of tartar, and its concentration is 40～43Be.

Add the hot water dilution and also carry out filter 23 while hot in the resultant that comprises solid B and liquid C, filtration temperature is 50～70 ℃, in case produce crystallization in filtration procedure, the concentration of filtrate D is 20～25Be.Filter residue B promptly produces active silica after washing 4, the water for cleaning amount of filter residue B is the dried slag of 1.5m/ ton.It is 18～20Be that filtrate D mixes 5 back concentration with the washings E that cleans for the first time filter residue B, and through inspissation to 32～36Be post crystallization 6, separation 7, crystallization temperature at end is 20 ± 5 ℃.Isolate is filtrate F and crystalline solid G, and filtrate F is an alum liquor, and further Tai-Ace S 150 is produced in inspissation crystallization 8.

During crystalline solid G moved into and still, weight such as addings are in the water of solid G, and heating makes it become Solution H 9, add in Solution H then in the bicarbonate of ammonia and 10, and reaction 10 finishes generation liquid I and solid J when pH value is 6.5～7.With liquid I and solid J filtering separation 11, solid J is dried after washing 12 and is made aluminium hydroxide, filtrate I and the washings K mixing 13 of cleaning solid J for the first time, the ratio of vitriolate of tartar and ammonium sulfate is in the mixed solution: 3: 8～9, vitriolate of tartar nitrogenous fertilizer L is promptly produced in its inspissation crystallization 14.

The utilization ratio of aluminium is 94% in the technology of the present invention, potassium extraction yield 90%, and the utilization ratio of silicon is 99.99%, raw ore utilization ratio nearly 100%.Illite raw material per ton can be produced potassium-nitrogen fertilizer 650kg, K2O 〉=11% wherein, N 〉=15%; Ignition dope level aluminium hydroxide product 200kg; Tai-Ace S 150 product 1400kg, Al2O 〉=15.7% wherein, Fe2O3＜0.35pd; Active silica 500kg.

The present invention need not to build stove and carries out high-temperature roasting owing to adopt sulfuric acid low temperature to decompose illite, and energy-saving effect is very obvious, less investment, and instant effect, technical process is simple, operation control easily, stable production process is reliable.Raw ore utilization ratio of the present invention is nearly 100%, and no mine tailing, pollution-free has multiple by-product, fully utilizes effective.The present invention adopts the illite of very easily exploiting in the many places of China as the raw material of producing potash fertilizer, has promptly enlarged the industrial raw material kind of potash fertilizer, also is simultaneously to illitic further increment exploitation.

Claims

1. produce the method for potassium-nitrogen fertilizer with illite for one kind, it is characterized in that:

A is with illite (K, H ₂O) A1 ₂[AlSi ₃O10] (H ₂O, OH) ₂For raw material with its pulverizing (1), make powder (A);

B, powder (A) is dropped in the reactor, the sulfuric acid of adding 50～60%, the sulfuric acid add-on is: 92% sulfuric acid: powder (A)=1: 1, reaction (2) under agitation condition, 135～145 ℃ of temperature of reaction, reaction pressure 0.3～0.4Mpa, 175～185 minutes reaction times, react to pH value be 1～2 o'clock, add Al ₂O ₃Transferring pH value is that 3 afterreactions (2) finish, and generates solid (B) and liquid (C);

C, in the resultant that comprises solid (B) and liquid (C), add the hot water dilution and filter (3), filter residue (B) is promptly produced active silica after washing (4), filtrate (D) is mixed (5) back inspissation crystallization (6) with the washings (E) that cleans for the first time filter residue (B), is separated (7), isolate is filtrate (F) and crystalline solid (G), and filtrate (F) further inspissation crystallization (8) is produced Tai-Ace S 150;

D, during crystalline solid (G) moved into and still, weight such as adding are in the water of solid (G), heating makes it become solution (H) (9), add bicarbonate of ammonia neutralization (10) then in solution (H), reaction (10) finishes when pH value is 6.5～7, generates liquid (I) and solid (J);

E, with liquid (I) and solid (J) filtering separation (11), solid (J) is made aluminium hydroxide through washing (12), and filtrate (I) and washings (K) mixing (13) of cleaning solid (J) are for the first time produced potassium-nitrogen fertilizer (L) through condensing crystal (14).

2. according to the method for producing potassium-nitrogen fertilizer described in the claim 1, it is characterized in that wherein said liquid (C) concentration is 40～43Be, filtrate (D) concentration is 20～25Be, 50～70 ℃ of filtration temperatures, and the water for cleaning amount of filter residue (B) is the dried slag of 1.5m/ ton.

3. according to the method for producing potassium-nitrogen fertilizer described in claim 1 and 3, it is characterized in that, it is 18～20Be that wherein said filtrate (D) is mixed back concentration with the washings (E) that partly cleans filter residue (B), inspissation to 32～36Be post crystallization (6), and the whole temperature of crystallization is 20 ± 5 ℃.