CN102180451A - Method for preparing magnesium hydrogen phosphate trihydrate from boric sludge and coproducing calcium hydroxide and sodium chloride - Google Patents
Method for preparing magnesium hydrogen phosphate trihydrate from boric sludge and coproducing calcium hydroxide and sodium chloride Download PDFInfo
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- CN102180451A CN102180451A CN2010105563917A CN201010556391A CN102180451A CN 102180451 A CN102180451 A CN 102180451A CN 2010105563917 A CN2010105563917 A CN 2010105563917A CN 201010556391 A CN201010556391 A CN 201010556391A CN 102180451 A CN102180451 A CN 102180451A
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Abstract
The invention discloses a method for preparing magnesium hydrogen phosphate trihydrate from boric sludge and coproducing calcium hydroxide and sodium chloride, relating to the treatment and integrated utilization of three wastes, i.e., waste water, waste gas and waste residue, in the inorganic chemical industry. The magnesium hydrogen phosphate trihydrate and the calcium hydroxide and the sodium chloride are prepared through performing a process of acid treatment and recovery and a process of synthesis and purification on the boric sludge. The process of acid treatment and recovery comprises the following steps of: heating the boric sludge by using vapor, separating solid from liquid by using a spin-drying centrifuge so as to obtain filtrate with boric acid primarily, wherein the filtrate is used for additional deep processing; reacting the magnesium oxide in a filter cake of the boric sludge with hydrochloric acid in a first corrosion-resistant reactor to produce the hydrate of magnesium chloride, calcium chloride and minute quantity of manganese chloride; and filtering to obtain a filter cake of silicon dioxide, wherein the filter cake of silicon dioxide is used for additional deep processing. The process of synthesis and purification comprises the following steps of: removing impurities and purifying in clarified filtrate by using right amount of magnesium hydroxide, and filtering to obtain a pure clarified solution of magnesium chloride dehydrate; reacting the obtained clarified magnesium chloride with disodium hydrogen phosphate in a second corrosion-resistant reactor; and heating and drying to obtain the product, i.e., magnesium hydrogen phosphate trihydrate. The economic benefit for treatment of waste boric sludge is improved.
Description
Technical field
The present invention relates to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly a kind of method that is equipped with secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge.
Background technology
Boron mud is with szaibelyite (2MgOB
2O
3H
2O) be raw material, by roasting, pulverizing, mix, take the carbon water law to produce borax (Na with soda ash
2B
4O
710H
2O), remaining solid waste after washing, crystallisation process extract borax.Produce one ton of borax and can produce 4 tons of boron mud, a borax plant that produces 8000 tons per year, can produce boron mud every year is 3.2 ten thousand tons.Because the quantity discharged of boron mud is bigger, the multiple comprehensive Utilization Ways of present domestic employing except that producing Magnesium Carbonate Light 41-45 and magnesium oxide and plastic and rubber filler, also has the coal of producing boron magnesium phosphorus composite fertilizer, making honeycomb briquette reinforced and do architectural borax etc.
Magnesium in the boron mud generally all is that the form with magnesiumcarbonate exists, and is sometimes also different and difference arranged along with the mineral products of szaibelyite.The component of producing the boron mud of Magnesium Carbonate Light 41-45 is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
One should improve constantly the value of output object to the utilization of boron mud, and some markets of output product in short supply, that added value is big is to improve the economic benefit that boron mud utilizes.
Its two, well-known, the utilization of boron mud is relevant with magnesium.Magnesium is subjected to people's attention to the effect of organism in recent years.That magnesium has is lax, the effect of expansion muscle, blood vessel, is indispensable mineral substance to the mankind.In recent years, magnesium significantly reduces in food precision work, so occurs the insufficient situation of magnesium in people's the diet easily, and therefore, the food of strengthen magnesium is subjected to people's welcome.In the food of strengthen magnesium, often use secondary magnesium phosphate.Secondary magnesium phosphate is mended the magnesium except being used for food, still is a kind of use fine chemical product widely.
Summary of the invention
The present invention is intended at the utilization of boron mud and the market requirement, and a kind of method that is equipped with secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge is provided.
To achieve these goals, be equipped with the technical scheme of method of secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge as follows in the present invention.
Be equipped with the method for secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge, boron mud makes secondary magnesium phosphate three water things by acid treatment recovery and synthesizing and purifying technology, simultaneously co-producing calcium hydroxide and sodium-chlor:
Technology is reclaimed in described acid treatment: boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with the liquid-solid separation of drying whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then; Magnesium oxide in the filter cake boron mud and hydrochloric acid react in first corrosion-resistant reactor by the mass ratio 1 of pure substance: 1.63-2.03, and stirring issues biochemical reaction blowing slowly; Reaction generates the Manganous chloride tetrahydrate of hydrate, calcium chloride and the minute quantity of magnesium chloride; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; Clarifying filtrate is done further purifying;
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution; The clarification magnesium chloride that obtains and the sodium hydrogen phosphate mass ratio 1 by pure substance: 1.63-2.03 reacts in second corrosion-resistant reactor; Under stirring slowly, generate seven water secondary magnesium phosphates and sodium-chlor mixing solutions; Filtration obtain filter cake through the washing drying, drying and crushing, checking the weight is packaged to be seven water secondary magnesium phosphate products; The continuation heat drying dries by the fire four crystal water molecules and obtains three water secondary magnesium phosphate products; The clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, and when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain the sodium chloride crystal product.
The used boron mud of the present invention is for producing the boron mud of Magnesium Carbonate Light 41-45, and its component is such: magnesium oxide, silicon-dioxide, carbonic acid gas, boron oxide, calcium oxide, manganese oxide also have moisture content.Certainly, other boron mud of similar components also can be suitable for the present invention's the method for preparing secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor.
Chemical equation of the present invention is:
MgO+2HCl＝＝＝＝MgCl
2+H
2O
CaO+2HCl＝＝＝＝CaCl
2+H
2O
CaCl
2+Mg(OH)
2＝＝＝＝MgCl
2+Ca(OH)
2
MnO+2HCl＝＝＝＝MnCl
2+H
2O
MnCl
2+Mg(OH)
2＝＝＝＝MgCl
2+Mn(OH)
2
MgCl
2+Na
2HPO
3+3H
2O＝＝＝＝MgHPO3·3H
2O+2NaCl
Beneficial effect of the present invention is: one, and provide a kind of and be equipped with the method for secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge, open up an approach for effectively handling boron mud waste material.Its two, preparation comprises secondary magnesium phosphate, calcium hydroxide and sodium-chlor, the bigger best-selling product of a kind of economic worth of secondary magnesium phosphate has wherein improved the economic benefit of handling boron mud waste material.Its three, less investment, particularly suitable to the boron mud of used boron mud of process for producing Magnesium Carbonate Light 41-45 and similar components, we can say and opened up a new road.Its four, the purity height of preparation, quality is guaranteed.
Embodiment
Embodiment one
Be equipped with the method for secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge, boron mud makes secondary magnesium phosphate three water things by acid treatment recovery and synthesizing and purifying technology, simultaneously co-producing calcium hydroxide and sodium-chlor:
Technology is reclaimed in described acid treatment: get 500 kilograms in boron mud (wherein containing magnesium oxide 38%), boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with the liquid-solid separation of drying whizzer, obtain sending to deep processing separately based on the filtrate of boric acid then; Magnesium oxide in the filter cake boron mud and hydrochloric acid react on first corrosion-resistant reactor by the mass ratio of pure substance 1: 1.63, issue biochemical reaction stirring slowly; Reaction generates the hydrate of 404 kilograms of magnesium chlorides, and other component generates the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; Clarifying filtrate is done further purifying;
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution; Obtain 404 kilograms clarification magnesium chlorides and sodium hydrogen phosphate are reacted on second corrosion-resistant reactor by the mass ratio of pure substance at 1: 1.63; Under stirring slowly, generate seven water secondary magnesium phosphates and sodium-chlor mixing solutions; Filtration obtain filter cake through the washing drying, drying and crushing, checking the weight is packaged to be seven water secondary magnesium phosphate products; The continuation heat drying dries by the fire four crystal water molecules and obtains 827.3 kilogram of three water secondary magnesium phosphate product; The clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, and when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain 611.5 kilograms sodium chloride crystal product.
The used boron mud of present embodiment is for producing the boron mud of Magnesium Carbonate Light 41-45, and its component is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Embodiment two
The method that is equipped with secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge, boron mud reclaims and is equipped with boric sludge the method synthesizing and purifying technology of magnesium hydroxide with coproduction calcium hydroxide and calcium chloride by acid treatment, make secondary magnesium phosphate three water things, simultaneously co-producing calcium hydroxide and sodium-chlor:
Technology is reclaimed in described acid treatment: get 500 kilograms in boron mud (wherein containing magnesium oxide 38%), boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with the liquid-solid separation of drying whizzer, obtain sending to deep processing separately based on the filtrate of boric acid then; Magnesium oxide in the filter cake boron mud and hydrochloric acid react on first corrosion-resistant reactor by the mass ratio of pure substance 1: 1.83, issue biochemical reaction stirring slowly; Reaction generates the hydrate of 453 kilograms of magnesium chlorides, and other component generates the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; Clarifying filtrate is done further purifying;
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution; Obtain 453 kilograms clarification magnesium chlorides and sodium hydrogen phosphate are reacted on second corrosion-resistant reactor by the mass ratio of pure substance at 1: 1.83; Under stirring slowly, generate seven water secondary magnesium phosphates and sodium-chlor mixing solutions; Filtration obtain filter cake through the washing drying, drying and crushing, checking the weight is packaged to be seven water secondary magnesium phosphate products; Continue heat drying and dry by the fire the three water secondary magnesium phosphate products that four crystal water molecules obtain 1041.5 kilograms; The clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, and when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain 769.8 kilograms sodium chloride crystal product.
The used boron mud of present embodiment is for producing the boron mud of Magnesium Carbonate Light 41-45, and its component is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Embodiment three
Be equipped with the method for secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge, boron mud makes secondary magnesium phosphate three water things by acid treatment recovery and synthesizing and purifying technology, simultaneously co-producing calcium hydroxide and sodium-chlor:
Technology is reclaimed in described acid treatment: get 500 kilograms in boron mud (wherein containing magnesium oxide 38%), boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with the liquid-solid separation of drying whizzer, obtain sending to deep processing separately based on the filtrate of boric acid then; Magnesium oxide in the filter cake boron mud and hydrochloric acid react on first corrosion-resistant reactor by the mass ratio of pure substance 1: 2.03, issue biochemical reaction stirring slowly; Reaction generates the hydrate of 503 kilograms of magnesium chlorides, and other component generates the Manganous chloride tetrahydrate that calcium chloride also has minute quantity; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; Clarifying filtrate is done further purifying;
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, the packing of checking the weight; And the magnesium chloride that generates has improved the concentration of original solution; Obtain 503 kilograms clarification magnesium chlorides and sodium hydrogen phosphate are reacted on second corrosion-resistant reactor by the mass ratio of pure substance at 1: 2.03; Under stirring slowly, generate seven water secondary magnesium phosphates and sodium-chlor mixing solutions; Filtration obtain filter cake through the washing drying, drying and crushing, checking the weight is packaged to be seven water secondary magnesium phosphate products; Continue heat drying and dry by the fire the three water secondary magnesium phosphate products that four crystal water molecules obtain 1282.9 kilograms; The clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, and when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain 948.2 kilograms sodium chloride crystal product.
The used boron mud of present embodiment is for producing the boron mud of Magnesium Carbonate Light 41-45, and its component is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Claims (2)
1. be equipped with the method for secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge, it is characterized in that: boron mud makes secondary magnesium phosphate three water things by acid treatment recovery and synthesizing and purifying technology, simultaneously co-producing calcium hydroxide and sodium-chlor:
Technology is reclaimed in described acid treatment: boron mud was kept 1-2 hour to 60-80 ℃ with steam heating, with the liquid-solid separation of drying whizzer, obtained sending to deep processing separately based on the filtrate of boric acid then; Magnesium oxide in the filter cake boron mud and hydrochloric acid react in first corrosion-resistant reactor by the mass ratio 1 of pure substance: 1.63-2.03, stir; Reaction generates hydrate, calcium chloride and the Manganous chloride tetrahydrate of magnesium chloride; Filtration obtains filter cake silicon-dioxide and sends to deep processing separately; Clarifying filtrate is done further purifying;
Described synthesizing and purifying technology is: the clear filtrate that described acid treatment recovery technology obtains is filtered and is obtained purified two aqueous magnesium chloride clear liquors at last with an amount of magnesium hydroxide impurity and purification; Calcium chloride and Manganous chloride tetrahydrate generate precipitation of hydroxide respectively and obtain calcium hydroxide and manganous hydroxide product respectively through washing drying, drying and crushing, sizing screening, packing; The clarification magnesium chloride that obtains and the sodium hydrogen phosphate mass ratio 1 by pure substance: 1.63-2.03 reacts in second corrosion-resistant reactor; Under agitation generate seven water secondary magnesium phosphates and sodium-chlor mixing solutions; Filtration obtains filter cake through washing drying, drying and crushing, being packaged to be seven water secondary magnesium phosphate products; The continuation heat drying dries by the fire four crystal water molecules and obtains three water secondary magnesium phosphate products; The clear filtrate that obtains is sent the underpressure distillation device to and is carried out underpressure distillation, and when solution reaches capacity concentration distillate being ejected through cooling has crystallization to separate out, through washing, dry, pulverize and obtain the sodium chloride crystal product.
2. the method that is equipped with secondary magnesium phosphate three water thing co-producing calcium hydroxides and sodium-chlor with boric sludge according to claim 1, it is characterized in that: described boron mud, contain magnesium oxide, silicon-dioxide, carbonic acid gas, boron oxide, calcium oxide, manganese oxide and moisture content in its component.
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|---|---|---|---|---|
| CN111533101A (en) * | 2020-04-07 | 2020-08-14 | 天津长芦海晶集团有限公司 | Method for preparing magnesium hydrogen phosphate trihydrate from brine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533101A (en) * | 2020-04-07 | 2020-08-14 | 天津长芦海晶集团有限公司 | Method for preparing magnesium hydrogen phosphate trihydrate from brine |
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Application publication date: 20110914 |