CN100360429C - Method for decomposing potash feldspar ore by low temperature wet process - Google Patents
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Abstract
The present invention relates to a method for decomposing potassium feldspar, particularly to a method for decomposing potassium feldspar in a low-temperature and wet decomposing method. The present invention is characterized in that the present invention comprises the following steps: 1) the potassium feldspar is pulverized into less than or equal to 200 meshes, hydrochloric acid and water are added to obtain a mother solution A and a filter cake A, and the mother solution A is prepared to obtain iron oxide red; 2) the filter cake A obtained in the step 1 is mixed with a fluoride mineral additive and the water, pulp is added into a reactor, SiF4 gas which escapes in the reaction is prepared to obtain white carbon black, the water is added into reaction products in the reactor, and the reaction products are filtered to obtain a filter solution C and CaSO4.2H2O; 3) the filtrate C is regulated by ammonia water to obtain a filter cake D and a mother solution D which is prepared to obtain potassium ammonium sulphate; 4) the water is added into the filter cake D of the third procedure to pulp the filter cake D, sulfuric acid is also added into the pulped filter cake D which is filtered to obtain a filter cake E and a filter solution E, and the filter cake E and the SiO2. nH2O prepared in the step 2 are uniformly mixed to obtain white carbon black; 5) ammonia water is added into the filter solution E filtered and obtained in the step 4 to obtain a filter cake F and a filter solution F which is prepared into aluminum hydroxide which is flame retardant. The method has the advantages of whole low temperature, low production cost and full resource utilization.
Description
Technical field
The present invention relates to a kind of method of decomposing potash feldspar ore.
Background technology
Potassium felspar sand (Potash feldspar) is a kind of K of containing
2O, Al
2O
3, SiO
2And contain Fe
2O
3Deng the natural mineral of impurity, molecular formula is K
2OAl
2O
36SiO
2Potassium felspar sand is the manufacture china main raw material of glaze of ceramic industry; Be a kind of of glass compound.Can increase enamelled viscosity and chemical stability, also can be used for making the enamel raw material, also can be used as the insulated electro ceramic material; It also is the raw material of making potash fertilizer.Also have many countries the batching of potassium felspar sand as cement raw material, and the recyclable K that gets
2SO
4Byproduct (the king chief editor that admonishes. chemical industry dictionary (third edition) [M]. Beijing: the .1992.602 of Chemical Industry Press).The domestic potassium felspar sand that develops is the earliest produced white cement and is loved to hear potash fertilizer plant by the Shanxi Province and carried out in 1980, and this factory adopts elevated temperature heat method potassium felspar sand to be decomposed K
2O overflows with the steam form, and solid K is reclaimed in cooling in tunnel furnace
2O, and make salt of wormwood, burned material then is used to be processed into white cement, and (Liu Guanglong, Yang Guolan appoint and set the mind on study, potassium felspar sand system salt of wormwood coproduction white fused cement [J], inorganic chemicals industry, 1988 (62): 15-19).In addition, Changsha chemical mine design and research institute is in application patent of invention in 1996, earlier potassium felspar sand and mineral acid and fluorochemical are reacted under atmospheric low-temperature, afterwards with solid materials through 500-750 ℃ of following high-temperature melting 1-3 hour, behind the product chemical industry, made potassium-ammonium sulfate again, active SiO
2And aluminum oxide, the potassium felspar sand rate of decomposition is 93% (potash feldspar ore wet method decomposition method, patent publication No. CN1138567).
At present, external research report aspect the potash feldspar ore comprehensive utilization is less.Domestic, though many people have carried out development and research, energy consumption is higher in the preparation process, especially the fluoride consumption is higher, comprehensive utilization of resources is not ideal enough, discharging in various degree more " three wastes " material, caused bigger pollution for environment or atmosphere.
Summary of the invention
The object of the present invention is to provide a kind of method of decomposing potash feldspar ore by low temperature wet process, the omnidistance low temperature of this method, production cost are low, resource is fully used.
To achieve these goals, technical scheme of the present invention is: the method for decomposing potash feldspar ore by low temperature wet process is characterized in that it comprises the steps:
1), feldspar in powder is broken to≤-200 orders, add weight concentration and be 30% hydrochloric acid and water and under 50-60 ℃, carry out stirring reaction, feldspar in powder: the weight ratio of hydrochloric acid is 1: 0.18-0.35, feldspar in powder: the weight ratio of water is 1: 0.9-1.1, react and filter after 1-2 hour, washing gets mother liquor A and filter cake A;
Mother liquor A adds ammoniacal liquor and is neutralized to pH=9.5-10, blast atmospheric oxidation at normal temperatures, oxidizing reaction 1.5-2.5 hour, the oxidation products therefrom is filtered, and use deionized water wash, get waste liquid B and filter cake B, with filter cake B in 120-125 ℃ of dry 2-3h, again at 650-670 ℃ of calcining 1h, be cooled to room temperature after, pulverize and promptly to obtain red iron oxide;
2), filter cake A that step 1) is obtained mixes with fluorochemical mineral additive, water, slurrying, the dry material of filter cake A: the weight ratio of fluorochemical mineral additive is 1: 2.4 0-2.50, the dry material of filter cake A: the weight ratio of water is 1: 1.8-2.2, slurry; Slurry is added in the reactor, and adding weight concentration is the sulfuric acid of 95-98%, and by the dry material of filter cake A: the vitriolic weight ratio is 1: 3.5-3.6 chooses sulfuric acid, reacts 1-3 hour, and temperature of reaction is 85-95 ℃, reacts effusion SiF
4Gas NH
4The F solution absorption forms (NH
4)
2SiF
6Solution, (NH
4)
2SiF
6Solution adds ammoniacal liquor and regulates pH=8.5-9.0, is settled out SiO
2NH
2O washs 3-5 time, filters, with the follow-up SiO that makes
2NH
2O mixing after drying is pulverized, and gets white carbon black;
Resultant of reaction in the reactor is added water, and the add-on of water is by the dry material of filter cake A: the weight ratio of water is 1: 1.5-1.6, and at 60-65 ℃, ageing is after 2 hours, the C and go out white depositions of filtering to get filtrate, white depositions is CaSO
4.2H
2O;
3), liquor C is regulated the pH value to 8.5-9.5 with ammoniacal liquor, carry out isolated by vacuum filtration, obtain filter cake D and mother liquor D; With mother liquor D vacuum concentration, crystallisation by cooling, centrifuge dehydration gets potassium-ammonium sulfate;
4), the filter cake D with step 3) adds water slurryization, and add the sulfuric acid that weight concentration is 15-18%, stirred 5-10 minute, the dry material of filter cake D: the weight ratio of water is 1: 2.3-3.0, the dry material of filter cake D: the vitriolic mass ratio is 1: 0.18-0.23, filter, filter cake E and filtrate E, filter cake E is with step 2) make SiO
2NH
2O mixes, and is dry then, pulverize, obtain white carbon black;
5), step 4) filtered the filtrate E obtain and adds ammoniacal liquor and regulate pH=8.5-9.5 after, under 60-70 ℃, stirred at a slow speed ageing 1-2 hour, after filtration, washing gets filter cake F and filtrate F, and filter cake F descended dry 1-2 hour at 105-110 ℃, pulverize, promptly make fire retardant aluminium hydroxide; The mother liquor D mixing vacuum concentration of filtrate F and step 3), crystallisation by cooling goes out potassium-ammonium sulfate.
Described fluorochemical mineral additive is the fluorite breeze, contains CaF
260-80%.
Only add fluorite breeze (cycles prepare) during first preparation, subsequent preparation then partly replaces the fluorite breeze with Neutral ammonium fluoride.
Of the present invention have following characteristics: (1) full low temperature (below 95 ℃) wet method decomposing of potassium feldspar breeze, and the main raw material fluoride can be recycled, and energy consumption is low, and preparation cost is low; (2) resource is fully used, the disposable 5 kinds of products (potassium-ammonium sulfate, white carbon black, aluminium hydroxide, red iron oxide and building materials gypsum) of preparing, and " three wastes " discharging is few; (3) made produce market situation is good, especially agricultural potassium sulfate ammonium, wherein K
2O content average out to 21.26% is a kind of good potassium nitrogen composite fertilizer material; (4) various quality producies all reach national correlated quality standard-required.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Implement starting material of the present invention and specification:
(1) K-feldspar K AlSi
3O
8Or K
2OAl
2O
36SiO
2(being crushed to-200 orders),
Form: K
2O average out to 10.5%,
SiO
2 ≥66％，
Al
2O
3 ≥15％，
Fe
2O
3 ≥3.8％。
(2) fluorite (CaF
2) (being crushed to-200 orders),
CaF
2Content 〉=70%.
(3) sulfuric acid (H
2SO
4) 98%.
(4) ammoniacal liquor (NH
3H
2O), nitrogen content 〉=25%.
(5) hydrochloric acid (HCl), HCl content 30%.
Embodiment 1:
As shown in Figure 1, the method for decomposing potash feldspar ore by low temperature wet process, it comprises the steps:
1), take by weighing 100g feldspar in powder (200 order), add water 100ml, add weight concentration and be 30% hydrochloric acid 18-20ml, stirred 1 hour down in 60 ℃, filter, washing (removes Cl
-), get mother liquor A and filter cake A; Mother liquor A is used to prepare red iron oxide, and it is that 30% ammoniacal liquor is neutralized to pH=9.5-10 that mother liquor A adds weight concentration, blasts atmospheric oxidation at normal temperatures, oxidizing reaction 1.5-2.5 hour, the oxidation products therefrom is filtered, and with deionized water wash to there not being Cl
-(being generally 3-4 time), liquid B and filter cake B, with filter cake B in 120-125 ℃ of dry 2-3h, again at 650-670 ℃ of calcining 1h, be cooled to room temperature after, pulverize and promptly to obtain red iron oxide (Fe
2O
3) 3.426g.
2), get the 120g filter cake A (contain moisture among the filter cake A, the dry material of filter cake A is 96.574g) of step 1) with 240g fluorite breeze (CaF
2Content is 70%) mix after, join in the reactor, after adding 200ml water and stirring, adding the 186ml weight concentration gradually is 98%H
2SO
4, reacted 2 hours, keep being reflected at 90 ℃ and carrying out effusion SiF
4Gas is at Venturi meter resorber NH
4The F solution absorption forms (NH
4)
2SiF
6Solution, (NH
4)
2SiF
6Solution adds ammoniacal liquor and regulates pH=8.5-9.0, is settled out SiO
2NH
2O stirs slaking 2 hours at a slow speed under 65 ℃, can guarantee that like this size of particles is even, and foreign matter content is few, is easy to washing and filtration; Wash 3-5 time, filter, with the follow-up SiO that makes
2NH
2O mixing after drying is pulverized, and gets white carbon black; Resultant of reaction in the reactor is added suitable quantity of water, and the add-on of water is by the dry material of filter cake A: the weight ratio of water is 1: 1.5-1.6, keep material at 60-65 ℃, and ageing is after 2 hours, and filter to get filtrate C and white depositions, white depositions are CaSO
42H
2O (can make the building materials gypsum uses).
3) be that 25% ammoniacal liquor is regulated pH value to 9.5, again with the liquor C weight concentration, filtering separation obtains filter cake D{ and contains SiO
2NH
2O and Al (OH)
3, and mother liquor D{ contain KNH
4SO
4; With mother liquor D vacuum concentration, crystallisation by cooling goes out potassium-ammonium sulfate 48g (K
2O is 21.26%);
4), with 125g filter cake D (contain moisture among the filter cake D, the dry material of filter cake D is 85g) with 200g water pulp again, and add the 105g sulfuric acid that weight concentration is 15-18%, stirred 5-10 minute, make Al (OH)
3Be converted into Al
2(SO
4)
3, and SiO
2NH
2O does not dissolve, after filtration and be washed till no SO
4 2-, getting filter cake E and filtrate E, filter cake E makes SiO with the front
2NH
2O mixes, and is dry then, pulverize, obtain the 65g white carbon black;
5), after the filtrate E that again filtration obtained adds ammoniacal liquor and regulate pH=9 ± 0.5, stir slaking 2 hours at a slow speed under 60-70 ℃, evenly stir at a slow speed simultaneously, can guarantee that like this size of particles is even, foreign matter content is few, is easy to washing and filters; After filtration, be washed till no SO
4 2-After, filter cake F and filtrate F, filter cake F 105-110 ℃ dry 2 hours down, pulverize, promptly make fire retardant aluminium hydroxide 19.26g; The mother liquor D mixing vacuum concentration of filtrate F and step 3), crystallisation by cooling goes out potassium-ammonium sulfate.Potassium felspar sand effectively decomposes utilization ratio and reaches 95%.
The white carbon black quality index sees Table 1, and the aluminium hydroxide quality index sees Table 2, and the red iron oxide quality index sees Table 3.
Embodiment 2:
Take by weighing the 100g potassium felspar sand, after the hydrochloric acid removal of impurities, mix, add the fluorinated ammonium and reclaim liquid (NH with the 10g fluorite
4F content is 20%) 250ml, added the 160ml sulfuric acid reaction again 1.5 hours, other process is made red iron oxide 3.506g respectively with embodiment 1, white carbon black 64.82g, fire retardant aluminium hydroxide 19.08g and potassium-ammonium sulfate 52g (K
2O is 20.83%).
Embodiment 3:
Take by weighing the 100g feldspar in powder, after salt acid treatment removal of impurities, add 5g fluorite breeze and 260ml (NH
4F is 19.5%), add 165ml sulfuric acid after mixing again, other operation steps is constant, makes red iron oxide 3.61g respectively, white carbon black 66.25g, aluminium hydroxide 19.42g, potassium-ammonium sulfate 53.06g (K
2O is 20.53%).
By above-mentioned three examples as can be known, no matter the potassium felspar sand breeze is to add the sulfuric acid decomposition or use NH with fluorite
4F decomposes with sulfuric acid, and the decomposition utilization ratio of ore all reaches 95%, illustrates that the present invention has good industrialized and utilizes prospect.
Table 1. is by the white carbon black quality index of the present invention's preparation
| Index name | GB10517-89 | The present technique average content |
| SiO 2The BET specific surface area/(m of content DBP oil-absorption(number)/(ml/100g) 2/ g) the total iron-holder of the total manganese content of residue on sieve (45 μ m)/% heating loss/total copper content of % burning decrement/% pH value/(mg/Kg)/(mg/Kg)/(mg/Kg) | ≥90 200～350 ≥71 0.5 4.0～8.0 ≤7.0 5.0～8.0 ≤30 ≤50 ≤1000 | 93.56 do not survey 75 0.43 5.2 6.1 7.6 12 23 216 |
Table 2. prepares fire retardant aluminium hydroxide quality index by the present invention
| Index name | Q/HG-288-85 (Chinese Enterprise) | Clear and the Electronics Co., Ltd (Japan) of Japan | Average content of the present invention |
| Than whiteness % free water content % acidity fineness (325 order) % median size μ m Al (OH) 3％ | ≥93 ≤0.45 9.2±0.5 ≥96 | 1～25 99.5～99.8 | 95 0.38 9.26 96 12 99.62 |
Main fire-retardant with doing in plastics and the rubber item, press down the cigarette effect.
Table 3. is by the red iron oxide quality index of the present invention's preparation
| Index name | HO 01-04Index | Average content of the present invention | |
| First grade | Qualified | ||
| Iron level is (with Fe 2O 3Meter, 105 ℃ of dryings) 105 ℃ of volatile matter % of % water solubles % water soluble chloride and vitriol are (with Cl -And SO 4 2Meter) existence of % residue on sieve (63 μ m) % water extract acid-base value ml water slurry pH value oil absorption g/100g plumbous chromate TC (in CaO) % color (with the standard sample ratio) relative color strength (with the standard sample ratio) % organic coloring thing | 〉=95≤1.0≤0.3≤0.2≤0.3≤20 5～7 15～25 feminine gender≤0.3 is similar to-little 〉=95 feminine genders | 90 1.5 0.5 0.3 0.5 20 5～7 15～25 feminine genders 0.3 are 90 feminine genders slightly | 97.21 0.96 0.27 0.18 0.31 13.6 6.5 16 negative 0.18 approximate 96 feminine genders |
Embodiment 4:
The method of decomposing potash feldspar ore by low temperature wet process, it comprises the steps:
1), feldspar in powder is broken to≤200 orders, add weight concentration and be 30% hydrochloric acid and water and under 50 ℃, carry out stirring reaction (oxide impurities of non-ferrous metals such as deironing), feldspar in powder: the weight ratio of hydrochloric acid is 1: 0.18, feldspar in powder: the weight ratio of water is 1: 0.9, react and filter after 1 hour, washing (removes Cl
-), get mother liquor A and filter cake A;
Mother liquor A is used to prepare red iron oxide, and it is that 30% ammoniacal liquor is neutralized to pH=9.5 that mother liquor A adds weight concentration, blasts atmospheric oxidation at normal temperatures, and oxidizing reaction 1.5 hours is filtered the oxidation products therefrom, and with deionized water wash to there not being Cl
-(being generally 3-4 time), waste liquid B and filter cake B, with filter cake B in 120 ℃ of dry 2h, again at 650 ℃ of calcining 1h, be cooled to room temperature after, pulverize and promptly to obtain red iron oxide;
2), filter cake A that step 1) is obtained mixes with fluorochemical mineral additive, water, slurrying, described fluorochemical mineral additive is the fluorite breeze, contains CaF
260-80%, the dry material of filter cake A: the weight ratio of fluorochemical mineral additive is 1: 2.40, the dry material of filter cake A: the weight ratio of water is 1: 1.8, gets slurry; Slurry is added in the corrosion-resistant stirred reactor, adds weight concentration and be 95% sulfuric acid, and by the dry material of filter cake A: the vitriolic weight ratio is to choose sulfuric acid at 1: 3.5, reacts 1 hour, and temperature of reaction is 85 ℃, reacts effusion SiF
4Gas NH
4The F solution absorption forms (NH
4)
2SiF
6Solution, (NH
4)
2SiF
6Solution adds ammoniacal liquor and regulates pH=8.5, is settled out SiO
2NH
2O stirs slaking 2 hours at a slow speed under 65 ℃, can guarantee that like this size of particles is even, and foreign matter content is few, is easy to washing and filtration; Wash 3 times, filter, with the follow-up SiO that makes
2NH
2O mixing after drying is pulverized, and gets white carbon black;
Resultant of reaction in the corrosion-resistant stirred reactor is added water, and the add-on of water is by the dry material of filter cake A: the weight ratio of water is 1: 1.5, and at 60 ℃, ageing is after 2 hours, the C and go out white depositions of filtering to get filtrate, and white depositions is CaSO
42H
2O (can make the building materials gypsum uses);
3), liquor C is regulated pH value to 8.5 with ammoniacal liquor, carry out isolated by vacuum filtration, obtain filter cake D{ and contain SiO
2NH
2O and Al (OH)
3, and mother liquor D{ contain KNH
4SO
4; With mother liquor D vacuum concentration, crystallisation by cooling, centrifuge dehydration gets potassium-ammonium sulfate;
4), the filter cake D of step 3) is added water slurryization, and to add weight concentration be 15% sulfuric acid, stirred 5-10 minute, the dry material of filter cake D: the weight ratio of water is 1: 2.3, the dry material of filter cake D: the vitriolic mass ratio is 1: 0.18, filters, filter cake E and filtrate E, filter cake E is with step 2) make SiO
2NH
2O mixes, and is dry then, pulverize, obtain white carbon black;
5), step 4) filtered the filtrate E obtain and adds ammoniacal liquor and regulate pH=8.5 after, under 60 ℃, stir ageing 1 hour at a slow speed, after filtration, washing is to there not being SO
4 2-After, filter cake F and filtrate F, filter cake F 105 ℃ dry 1 hour down, pulverize, promptly make fire retardant aluminium hydroxide; The mother liquor D mixing vacuum concentration of filtrate F and step 3), crystallisation by cooling goes out potassium-ammonium sulfate.
Embodiment 5:
The method of decomposing potash feldspar ore by low temperature wet process, it comprises the steps:
1), feldspar in powder is broken to≤200 orders, add weight concentration and be 30% hydrochloric acid and water and under 60 ℃, carry out stirring reaction (oxide impurities of non-ferrous metals such as deironing), feldspar in powder: the weight ratio of hydrochloric acid is 1: 0.35, feldspar in powder: the weight ratio of water is 1: 1.1, react and filter after 2 hours, washing (removes Cl
-), get mother liquor A and filter cake A;
Mother liquor A is used to prepare red iron oxide, and it is that 30% ammoniacal liquor is neutralized to pH=10 that mother liquor A adds weight concentration, blasts atmospheric oxidation at normal temperatures, and oxidizing reaction 2.5 hours is filtered the oxidation products therefrom, and with deionized water wash to there not being Cl
-(being generally 3-4 time), waste liquid B and filter cake B, with filter cake B in 125 ℃ of dry 3h, again at 670 ℃ of calcining 1h, be cooled to room temperature after, pulverize and promptly to obtain red iron oxide;
2), filter cake A that step 1) is obtained mixes with fluorochemical mineral additive, water, slurrying, described fluorochemical mineral additive is the fluorite breeze, contains CaF
260-80%, the dry material of filter cake A: the weight ratio of fluorochemical mineral additive is 1: 2.50, the dry material of filter cake A: the weight ratio of water is 1: 2.2, gets slurry; Slurry is added in the corrosion-resistant stirred reactor, adds weight concentration and be 98% sulfuric acid, and by the dry material of filter cake A: the vitriolic weight ratio is to choose sulfuric acid at 1: 3.6, reacts 3 hours, and temperature of reaction is 95 ℃, reacts effusion SiF
4Gas NH
4The F solution absorption forms (NH
4)
2SiF
6Solution, (NH4)
2SiF
6Solution adds ammoniacal liquor and regulates pH=9.0, is settled out SiO
2NH
2O stirs slaking 2 hours at a slow speed under 65 ℃, can guarantee that like this size of particles is even, and foreign matter content is few, is easy to washing and filtration; Wash 5 times, filter, with the follow-up SiO that makes
2NH
2O mixing after drying is pulverized, and gets white carbon black;
Resultant of reaction in the corrosion-resistant stirred reactor is added water, and the add-on of water is by the dry material of filter cake A: the weight ratio of water is 1: 1.6, and at 65 ℃, ageing is after 2 hours, the C and go out white depositions of filtering to get filtrate, and white depositions is CaSO
42H
2O (can make the building materials gypsum uses);
3), liquor C is regulated pH value to 9.5 with ammoniacal liquor, carry out isolated by vacuum filtration, obtain filter cake D{ and contain SiO
2NH
2O and Al (OH)
3, and mother liquor D{ contain KNH
4SO
4; With mother liquor D vacuum concentration, crystallisation by cooling, centrifuge dehydration gets potassium-ammonium sulfate;
4), the filter cake D of step 3) is added water slurryization, and to add weight concentration be 18% sulfuric acid, stirred 10 minutes, the dry material of filter cake D: the weight ratio of water is 1: 3.0, the dry material of filter cake D: the vitriolic mass ratio is 1: 0.23, filters, filter cake E and filtrate E, filter cake E is with step 2) make SiO
2NH
2O mixes, and is dry then, pulverize, obtain white carbon black;
5), step 4) filtered the filtrate E obtain and adds ammoniacal liquor and regulate pH=9.5 after, under 70 ℃, stir ageing 2 hours at a slow speed, after filtration, washing is to there not being SO
4 2-After, filter cake F and filtrate F, filter cake F 110 ℃ dry 2 hours down, pulverize, promptly make fire retardant aluminium hydroxide; The mother liquor D mixing vacuum concentration of filtrate F and step 3), crystallisation by cooling goes out potassium-ammonium sulfate.
Claims (2)
1. the method for decomposing potash feldspar ore by low temperature wet process is characterized in that it comprises the steps:
1), feldspar in powder is broken to≤200 orders, add weight concentration and be 30% hydrochloric acid and water and under 50-60 ℃, carry out stirring reaction, feldspar in powder: the weight ratio of hydrochloric acid is 1: 0.18-0.35, feldspar in powder: the weight ratio of water is 1: 0.9-1.1, react and filter after 1-2 hour, washing gets mother liquor A and filter cake A;
Mother liquor A adds ammoniacal liquor and is neutralized to pH=9.5-10, blast atmospheric oxidation at normal temperatures, oxidizing reaction 1.5-2.5 hour, the oxidation products therefrom is filtered, and use deionized water wash, get waste liquid B and filter cake B, with filter cake B in 120-125 ℃ of dry 2-3h, again at 650-670 ℃ of calcining 1h, be cooled to room temperature after, pulverize and promptly to obtain red iron oxide;
2), filter cake A that step 1) is obtained mixes with fluorochemical mineral additive, water, slurrying, the dry material of filter cake A: the weight ratio of fluorochemical mineral additive is 1: 2.40-2.50, the dry material of filter cake A: the weight ratio of water is 1: 1.8-2.2, slurry; Slurry is added in the reactor, and adding weight concentration is the sulfuric acid of 95-98%, and by the dry material of filter cake A: the vitriolic weight ratio is 1: 3.5-3.6 chooses sulfuric acid, reacts 1-3 hour, and temperature of reaction is 85-95 ℃, reacts effusion SiF
4Gas NH
4The F solution absorption forms (NH
4)
2SiF
6Solution, (NH
4)
2SiF
6Solution adds ammoniacal liquor and regulates pH=8.5-9.0, is settled out SiO
2NH
2O washs 3-5 time, filters, with the follow-up SiO that makes
2NH
2O mixing after drying is pulverized, and gets white carbon black;
Resultant of reaction in the reactor is added water, and the add-on of water is by the dry material of filter cake A: the weight ratio of water is 1: 1.5-1.6, and at 60-65 ℃, ageing is after 2 hours, the C and go out white depositions of filtering to get filtrate, white depositions is CaSO
42H
2O;
3), liquor C is regulated the pH value to 8.5-9.5 with ammoniacal liquor, carry out isolated by vacuum filtration, obtain filter cake D and mother liquor D; With mother liquor D vacuum concentration, crystallisation by cooling, centrifuge dehydration gets potassium-ammonium sulfate;
4), the filter cake D with step 3) adds water slurryization, and add the sulfuric acid that weight concentration is 15-18%, stirred 5-10 minute, the dry material of filter cake D: the weight ratio of water is 1: 2.3-3.0, the dry material of filter cake D: the vitriolic mass ratio is 1: 0.18-0.23, filter, filter cake E and filtrate E, filter cake E is with step 2) make SiO
2NH
2O mixes, and is dry then, pulverize, obtain white carbon black;
5), step 4) filtered the filtrate E obtain and adds ammoniacal liquor and regulate pH=8.5-9.5 after, under 60-70 ℃, stirred at a slow speed ageing 1-2 hour, after filtration, washing gets filter cake F and filtrate F, and filter cake F descended dry 1-2 hour at 105-110 ℃, pulverize, promptly make fire retardant aluminium hydroxide; The mother liquor D mixing vacuum concentration of filtrate F and step 3), crystallisation by cooling goes out potassium-ammonium sulfate.
2. the method for decomposing potash feldspar ore by low temperature wet process according to claim 1, it is characterized in that: described fluorochemical mineral additive is the fluorite breeze, contains CaF
260-80%.
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| CN100360429C true CN100360429C (en) | 2008-01-09 |
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| CN103449882A (en) * | 2013-08-26 | 2013-12-18 | 成都化工股份有限公司 | Method for producing ammonium potassium compound fertilizer by utilizing potassium salt extracted from potassium feldspar |
| CN103539177A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technology for preparing aluminum hydroxide by use of potassium feldspar |
| CN103601229B (en) * | 2013-11-01 | 2015-04-01 | 青岛星火化工技术有限公司 | Method for preparation of chemical raw materials by using of potassium-containing shale |
| CN103787421B (en) * | 2013-12-24 | 2014-12-17 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of sylvine-containing rock |
| CN103708524B (en) * | 2013-12-24 | 2014-12-17 | 贵州远盛钾业科技有限公司 | Method for preparing chemical materials by decomposing potassium-bearing rock by fluorosilicic acid cycling method |
| CN105060350A (en) * | 2015-08-04 | 2015-11-18 | 贵州远盛钾业科技有限公司 | Production method of iron oxide by utilizing potassium-bearing rock |
| CN106631284A (en) * | 2017-01-04 | 2017-05-10 | 山西农业大学 | Preparation method of citrate-soluble potassium inorganic compound fertilizer |
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| CN1557781A (en) * | 2004-02-04 | 2004-12-29 | 薛彦辉 | Low temperature decomposition method for potassium feldspar |
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| Title |
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| 钾长石－萤石－硫酸体系中分解钾长石的探讨. 薛彦辉等.化学与生物工程，第2卷. 2004 * |
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