CN102180450A - Method for preparing magnesium hydrogen phosphate anhydride and co-producing calcium hydroxide and sodium chloride with boron mud - Google Patents
Method for preparing magnesium hydrogen phosphate anhydride and co-producing calcium hydroxide and sodium chloride with boron mud Download PDFInfo
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- CN102180450A CN102180450A CN2010105563809A CN201010556380A CN102180450A CN 102180450 A CN102180450 A CN 102180450A CN 2010105563809 A CN2010105563809 A CN 2010105563809A CN 201010556380 A CN201010556380 A CN 201010556380A CN 102180450 A CN102180450 A CN 102180450A
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Abstract
The invention provides to a method for preparing magnesium hydrogen phosphate anhydride and co-producing calcium hydroxide and sodium chloride with boron mud, relating to inorganic chemical three-waste treatment and comprehensive utilization. The method is characterized in that the magnesium hydrogen phosphate anhydride is prepared from the boron mud through an acid treatment recovery process and a synthesis and purification process, and simultaneously calcium hydroxide and sodium chloride are co-produced, wherein the acid treatment recovery process comprises the following steps: heating the boron mud with steam, carrying out solid-liquid separation by virtue of a drying centrifugal machine so as to obtain a filtrate with boric acid as a main component, and then feeding the filtrate for additionally deep processing; and reacting magnesium oxide in a filter cake boron mud with hydrochloric acid in a first corrosion resisting reactor so as to generate magnesium chloride hydrate, calcium chloride and an extremely small quantity of manganese chloride, filtering so as to obtain filter cake silica, and feeding the filter cake for additionally deep processing. The synthesis and purification process comprises the following steps: carrying out impurity removal and purification on a clear filtrate by utilizing a proper amount of magnesium hydroxide, and filtering so as to obtain a purified magnesium chloride dihydrate clear liquid; and reacting the obtained magnesium chloride with dibastic sodium phosphate in a second corrosion resistance reactor, heating and drying so as to obtain the magnesium hydrogen phosphate anhydride. By using the method, the economic benefits of treating boron mud waste materials are 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 anhydride co-producing calcium hydroxide 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 to the utilization and the market requirement at boron mud waste material, and a kind of method that is equipped with secondary magnesium phosphate anhydride co-producing calcium hydroxide and sodium-chlor with boric sludge is provided.
To achieve these goals, prepare the technical scheme of method of secondary magnesium phosphate anhydride co-producing calcium hydroxide and sodium-chlor with boron mud waste material as follows in the present invention.
Be equipped with the method for secondary magnesium phosphate anhydride co-producing calcium hydroxide and sodium-chlor with boric sludge, boron mud makes the secondary magnesium phosphate anhydride 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; Continuing heat drying dries by the fire whole crystal water molecule temperature and reaches 170 ℃ and obtain anhydrous phosphoric acid hydrogen magnesium 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 anhydride co-producing calcium hydroxide 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 anhydride co-producing calcium hydroxide and sodium-chlor with boric sludge, boron mud makes the secondary magnesium phosphate anhydride 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; Continuing heat drying dries by the fire whole crystal water molecule temperature and reaches 170 ℃ and obtain 545.1 kilograms of anhydrous phosphoric acid hydrogen magnesium 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 611.5 kilograms of sodium chloride crystal products.
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
Be equipped with the method for secondary magnesium phosphate anhydride co-producing calcium hydroxide and sodium-chlor with boric sludge, boron mud makes the secondary magnesium phosphate anhydride 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: 1.83, 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; Continuing heat drying dries by the fire whole crystal water molecule temperature and reaches 170 ℃ and obtain 686.2 kilograms of anhydrous phosphoric acid hydrogen magnesium 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 769.8 kilograms of sodium chloride crystal products.
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 anhydride co-producing calcium hydroxide and sodium-chlor with boric sludge, boron mud makes the secondary magnesium phosphate anhydride 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; Continuing heat drying dries by the fire whole crystal water molecule temperature and reaches 170 ℃ and obtain 845.2 kilograms of anhydrous phosphoric acid hydrogen magnesium 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 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 anhydride co-producing calcium hydroxide and sodium-chlor with boric sludge, it is characterized in that, boron mud makes the secondary magnesium phosphate anhydride 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; 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 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; Continuing heat drying dries by the fire whole crystal water molecule temperature and reaches 170 ℃ and obtain anhydrous phosphoric acid hydrogen magnesium 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 anhydride co-producing calcium hydroxide 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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| CN2010105563809A CN102180450A (en) | 2010-11-23 | 2010-11-23 | Method for preparing magnesium hydrogen phosphate anhydride and co-producing calcium hydroxide and sodium chloride with boron mud |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055500A (en) * | 2017-03-08 | 2017-08-18 | 中国海洋大学 | Three water magnesium monohydrogen phosphates are prepared in non-aqueous system |
-
2010
- 2010-11-23 CN CN2010105563809A patent/CN102180450A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055500A (en) * | 2017-03-08 | 2017-08-18 | 中国海洋大学 | Three water magnesium monohydrogen phosphates are prepared in non-aqueous system |
| CN107055500B (en) * | 2017-03-08 | 2019-04-30 | 中国海洋大学 | Three water magnesium monohydrogen phosphates are prepared in non-aqueous system |
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Application publication date: 20110914 |