CN105883744A - Method for co-production of hydrous magnesium hydrogen phosphate, calcium hydrate and sodium chloride from boron mud - Google Patents
Method for co-production of hydrous magnesium hydrogen phosphate, calcium hydrate and sodium chloride from boron mud Download PDFInfo
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- CN105883744A CN105883744A CN201410478054.9A CN201410478054A CN105883744A CN 105883744 A CN105883744 A CN 105883744A CN 201410478054 A CN201410478054 A CN 201410478054A CN 105883744 A CN105883744 A CN 105883744A
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- magnesium
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- boron mud
- sodium chloride
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Abstract
The invention discloses a method for co-production of hydrous magnesium hydrogen phosphate, calcium hydrate and sodium chloride from boron mud and relates to inorganic chemical three-waste treatment and integrated utilization. The method comprises co-producing a magnesium hydrogen phosphate trihydrate, calcium hydrate and sodium chloride through acid treatment recovery and synthesis and purification. The acid treatment recovery process comprises that boron mud is subjected to steam heating and then is subjected to liquid-solid separation under action of a spin-drying centrifugal machine so that the filtrate mainly containing boric acid is obtained, the filtrate is deep processed, magnesium oxide of the filter cake and hydrochloric acid undergoes a reaction in a first corrosion-resistant reactor to produce a magnesium chloride hydrate, calcium chloride and minute quantity of manganese chloride, the products are filtered to obtain filter cake silica and the filter cake is deep processed. The synthesis and purification process comprises removing impurities in the clear filtrate through a proper amount of magnesium hydroxide, carrying out filtration to obtain a pure magnesium chloride dihydrate clear solution, carrying out a reaction process on the clear magnesium chloride and sodium hydrogen phosphate in a second corrosion-resistant reactor and carrying out heating drying to obtain a magnesium hydrogen phosphate trihydrate product. The method improves boron mud waste material treatment economic benefits.
Description
Technical field
The present invention relates to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly one boron mud produces water-bearing phosphate
Hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride.
Background technology
Boron mud is with boromagnesite (2MgO B2O3·H2O) it is raw material, is mixed with soda ash by roasting, pulverizing, take carbon water law
Produce borax (Na2B4O7·10H2O), remaining solid waste after washing, crystallization process extract borax.Producing one ton of borax can
Producing 4 tons of boron mud, a borax plant producing 8000 tons per year, can produce boron mud every year is 3.2 ten thousand tons.Owing to the discharge capacity of boron mud is relatively big,
The current multiple comprehensive Utilization Ways of domestic employing, in addition to producing light magnesium carbonate and magnesia and plastic and rubber filler, also produces boron
Mei Lin composite fertilizer, make honeycomb briquette coal charging and do architectural borax etc..
Magnesium in boron mud is typically all presented in magnesium carbonate, sometimes has difference also with the mineral products difference of boromagnesite.
The component of production light magnesium carbonate boron mud is such that magnesia and accounts for 38%, and silica accounts for 20%, and carbon dioxide accounts for 17%,
Boron oxide accounts for 3%, and calcium oxide accounts for 3%, and manganese oxide accounts for 0.11%, and other is moisture content.
One, should improve constantly the value of output object to the utilization of boron mud, product that some markets of output are in short supply, that added value is big,
To improve the economic benefit that boron mud utilizes.
They are two years old, it is well known that the utilization of boron mud is relevant with magnesium.Organism is acted on and being paid close attention to by people by magnesium in recent years.Magnesium
There is lax, expansion muscle and the effect of blood vessel, be indispensable mineral matter for the mankind.In recent years, magnesium is in food essence
Being greatly decreased in processing, therefore easily occur the situation that magnesium is not enough in the diet of people, therefore, the food of strengthening magnesium is by people
Welcome.In the food of strengthening magnesium, commonly used magnesium monohydrogen phosphate.Magnesium monohydrogen phosphate except mending in addition to magnesium in food, or
One uses fine chemical product widely.
Summary of the invention
It is contemplated that for the utilization of boron mud and the market demand, it is provided that a kind of produce water-bearing phosphate hydrogen magnesium coproduction hydroxide by boron mud
Calcium and the method for sodium chloride.
To achieve these goals, present invention boron mud production water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the skill of the method for sodium chloride
Art scheme is as follows.
Producing water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride by boron mud, boron mud is reclaimed by acid treatment and synthesizes pure
Metallization processes, prepares magnesium monohydrogen phosphate three water thing, co-producing calcium hydroxide and sodium chloride simultaneously:
Described acid treatment recovery process is: boron mud steam is heated to 61～81 DEG C and maintains 1.1～2.1 hours, then with getting rid of
Dry centrifuge solid-liquor separation, obtains the filtrate based on boric acid and sends to deep processing separately；Magnesia in filter cake boron mud is pressed with hydrochloric acid
The mass ratio 1: 1.61～2.04 of pure material meter, reacts in the first corrosion-resistant reactor, stirring slowly issue biochemical instead
Should；Reaction generates the hydrate of magnesium chloride, calcium chloride and minimal amount of manganese chloride；It is filtrated to get filter cake silica to send to separately
Deep processing；The filtrate of clarification is further purified；
Described synthesizing and purifying technique is: the clear filtrate that described acid treatment recovery process obtains is clean with appropriate magnesium hydroxide removal of impurities
Change, filter and finally obtain two pure aqueous magnesium chloride clarified solutions；It is scrubbed that calcium chloride and manganese chloride generate hydroxide precipitation respectively
Drying, drying and crushing, sizing screening, packaging of checking the weight respectively obtain calcium hydroxide and manganous hydroxide product；And the magnesium chloride generated
Improve the concentration of original solution；Clarification magnesium chloride and the dibastic sodium phosphate obtained mass ratio 1: 1.61～2.04 based on pure material
React in the second corrosion-resistant reactor；Seven water magnesium monohydrogen phosphates and sodium chloride mixed solution is generated under stirring slowly；It is filtrated to get
The scrubbed drying of filter cake, drying and crushing, checking the weight is packaged to be seven water magnesium monohydrogen phosphate products；Continue heat drying and bake out four crystallizations
Hydrone obtains three water magnesium monohydrogen phosphate products；The clear filtrate obtained is sent into decompression distiller and carries out decompression distillation, when solution reaches
Being ejected by distillate when saturated concentration cooled has a crystallization, scrubbed, dry, pulverize and obtain sodium chloride crystal product.
Boron mud used by the present invention is the boron mud producing light magnesium carbonate, and its component is such that magnesia, silica, dioxy
Change carbon, boron oxide, calcium oxide, manganese oxide, also moisture content.Certainly, other boron mud of similar components also can be suitable for the present invention it
Prepare magnesium monohydrogen phosphate three water thing co-producing calcium hydroxide and the method for sodium chloride.
The chemical equation of the present invention is:
MgO+2HCl=MgCl2+H2O
CaO+2HCl=CaCl2+H2O
CaCl2+Mg(OH)2=MgCl2+Ca(OH)2
MnO+2HCl=MnCl2+H2O
MnCl2+Mg(OH)2=MgCl2+Mn(OH)2
MgCl2+Na2HPO3+3H2O=MgHPO3·3H2O+2NaCl
The beneficial effects of the present invention is: one, it is provided that a kind of with boron mud production water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and chlorine
The method changing sodium, opens up an approach for effectively processing boric sludge waste.Its two, preparation include magnesium monohydrogen phosphate, calcium hydroxide and
Sodium chloride, the best-selling product that wherein a kind of economic worth of magnesium monohydrogen phosphate is bigger, improve the economic benefit processing boric sludge waste.Its
Three, small investment, especially suitable to the boron mud of boron mud and similar components used by process for producing light magnesium carbonate, it may be said that to open one
Tiao Xin road.Its four, the purity of preparation is high, and quality is guaranteed.
Detailed description of the invention
Embodiment one
Producing water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride by boron mud, boron mud is reclaimed by acid treatment and synthesizes pure
Metallization processes, prepares magnesium monohydrogen phosphate three water thing, co-producing calcium hydroxide and sodium chloride simultaneously:
Described acid treatment recovery process is: takes boron mud 500 kilograms (wherein containing magnesia 38%), is heated to by boron mud steam
61～81 DEG C maintain 1.1～2.1 hours, then with drying centrifuge solid-liquor separation, obtain the filtrate based on boric acid and send to separately
Deep processing；Magnesia in filter cake boron mud and the hydrochloric acid mass ratio 1: 1.63 based on pure material, reacts on the first corrosion-resistant reaction
Device, issues biochemical reaction in stirring slowly；Reaction generates the hydrate of 404 kilograms of magnesium chlorides, and other component generates calcium chloride
Also has minimal amount of manganese chloride；It is filtrated to get filter cake silica and sends to deep processing separately；The filtrate of clarification is further purified；
Described synthesizing and purifying technique is: the clear filtrate that described acid treatment recovery process obtains is clean with appropriate magnesium hydroxide removal of impurities
Change, filter and finally obtain two pure aqueous magnesium chloride clarified solutions；It is scrubbed that calcium chloride and manganese chloride generate hydroxide precipitation respectively
Drying, drying and crushing, sizing screening, packaging of checking the weight respectively obtain calcium hydroxide and manganous hydroxide product；And the magnesium chloride generated
Improve the concentration of original solution；Obtain 404 kilograms clarification magnesium chlorides and the dibastic sodium phosphate mass ratio 1: 1.63 based on pure material
React on the second corrosion-resistant reactor；Seven water magnesium monohydrogen phosphates and sodium chloride mixed solution is generated under stirring slowly；It is filtrated to get filter
The scrubbed drying of cake, drying and crushing, checking the weight is packaged to be seven water magnesium monohydrogen phosphate products；Continue heat drying and bake out four crystallizations water
Molecule obtains 827.3 kilogram of three water magnesium monohydrogen phosphate product；The clear filtrate obtained is sent into decompression distiller and carries out decompression distillation, when
Being ejected by distillate time solution reaches saturated concentration cooled has a crystallization, scrubbed, dry, pulverize and obtain 611.5
Kilogram sodium chloride crystal product.
Boron mud used by the present embodiment is the boron mud producing light magnesium carbonate, and its component is such that magnesia 38%, silica
20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Embodiment two
Producing water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride by boron mud, boron mud is reclaimed by acid treatment and uses boron mud
Prepare the method synthesizing and purifying technique of magnesium hydroxide with coproduction of calcium hydroxide and calcium chloride, prepare magnesium monohydrogen phosphate three water thing, coproduction simultaneously
Calcium hydroxide and sodium chloride:
Described acid treatment recovery process is: takes boron mud 500 kilograms (wherein containing magnesia 38%), is heated to by boron mud steam
61～81 DEG C maintain 1.1～2.1 hours, then with drying centrifuge solid-liquor separation, obtain the filtrate based on boric acid and send to separately
Deep processing；Magnesia in filter cake boron mud and the hydrochloric acid mass ratio 1: 1.83 based on pure material, reacts on the first corrosion-resistant reaction
Device, issues biochemical reaction in stirring slowly；Reaction generates the hydrate of 453 kilograms of magnesium chlorides, and other component generates calcium chloride
Also has minimal amount of manganese chloride；It is filtrated to get filter cake silica and sends to deep processing separately；The filtrate of clarification is further purified；
Described synthesizing and purifying technique is: the clear filtrate that described acid treatment recovery process obtains is clean with appropriate magnesium hydroxide removal of impurities
Change, filter and finally obtain two pure aqueous magnesium chloride clarified solutions；It is scrubbed that calcium chloride and manganese chloride generate hydroxide precipitation respectively
Drying, drying and crushing, sizing screening, packaging of checking the weight respectively obtain calcium hydroxide and manganous hydroxide product；And the magnesium chloride generated
Improve the concentration of original solution；Obtain 453 kilograms clarification magnesium chlorides and the dibastic sodium phosphate mass ratio 1: 1.83 based on pure material
React on the second corrosion-resistant reactor；Seven water magnesium monohydrogen phosphates and sodium chloride mixed solution is generated under stirring slowly；It is filtrated to get filter
The scrubbed drying of cake, drying and crushing, checking the weight is packaged to be seven water magnesium monohydrogen phosphate products；Continue heat drying and bake out four crystallizations water
Molecule obtains the three water magnesium monohydrogen phosphate products of 1041.5 kilograms；The clear filtrate obtained is sent into decompression distiller and carries out decompression distillation,
Being ejected by distillate when solution reaches saturated concentration time cooled has a crystallization, scrubbed, dry, pulverize and obtain 769.8
Kilogram sodium chloride crystal product.
Boron mud used by the present embodiment is the boron mud producing light magnesium carbonate, and its component is such that magnesia 38%, silica
20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Embodiment three
Producing water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride by boron mud, boron mud is reclaimed by acid treatment and synthesizes pure
Metallization processes, prepares magnesium monohydrogen phosphate three water thing, co-producing calcium hydroxide and sodium chloride simultaneously:
Described acid treatment recovery process is: takes boron mud 500 kilograms (wherein containing magnesia 38%), is heated to by boron mud steam
61～81 DEG C maintain 1.1～2.1 hours, then with drying centrifuge solid-liquor separation, obtain the filtrate based on boric acid and send to separately
Deep processing；Magnesia in filter cake boron mud and the hydrochloric acid mass ratio 1: 2.03 based on pure material, reacts on the first corrosion-resistant reaction
Device, issues biochemical reaction in stirring slowly；Reaction generates the hydrate of 503 kilograms of magnesium chlorides, and other component generates calcium chloride
Also has minimal amount of manganese chloride；It is filtrated to get filter cake silica and sends to deep processing separately；The filtrate of clarification is further purified；
Described synthesizing and purifying technique is: the clear filtrate that described acid treatment recovery process obtains is clean with appropriate magnesium hydroxide removal of impurities
Change, filter and finally obtain two pure aqueous magnesium chloride clarified solutions；It is scrubbed that calcium chloride and manganese chloride generate hydroxide precipitation respectively
Drying, drying and crushing, sizing screening, packaging of checking the weight respectively obtain calcium hydroxide and manganous hydroxide product；And the magnesium chloride generated
Improve the concentration of original solution；Obtain 503 kilograms clarification magnesium chlorides and the dibastic sodium phosphate mass ratio 1: 2.03 based on pure material
React on the second corrosion-resistant reactor；Seven water magnesium monohydrogen phosphates and sodium chloride mixed solution is generated under stirring slowly；It is filtrated to get filter
The scrubbed drying of cake, drying and crushing, checking the weight is packaged to be seven water magnesium monohydrogen phosphate products；Continue heat drying and bake out four crystallizations water
Molecule obtains the three water magnesium monohydrogen phosphate products of 1282.9 kilograms；The clear filtrate obtained is sent into decompression distiller and carries out decompression distillation,
Being ejected by distillate when solution reaches saturated concentration time cooled has a crystallization, scrubbed, dry, pulverize and obtain 948.2
Kilogram sodium chloride crystal product.
Boron mud used by the present embodiment is the boron mud producing light magnesium carbonate, and its component is such that magnesia 38%, silica
20%, carbon dioxide 17%, boron oxide 3%, calcium oxide 3%, manganese oxide 0.11%, other are moisture content.
Claims (2)
1. produce water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride by boron mud, it is characterised in that: boron mud by acid at
Reason reclaims and synthesizing and purifying technique, prepares magnesium monohydrogen phosphate three water thing, co-producing calcium hydroxide and sodium chloride simultaneously: described acid treatment is returned
Skill of knocking off is: boron mud steam is heated to 61～81 DEG C and maintains 1.1～2.1 hours, then with drying centrifuge solid-liquor separation,
Obtain the filtrate based on boric acid and send to deep processing separately；Magnesia in filter cake boron mud and the hydrochloric acid mass ratio 1 based on pure material:
1.61～2.04, react in the first corrosion-resistant reactor, stirring；Reaction generates the hydrate of magnesium chloride, calcium chloride and chlorination
Manganese；It is filtrated to get filter cake silica and sends to deep processing separately；The filtrate of clarification is further purified；Described synthesizing and purifying work
Skill is: the clear filtrate that described acid treatment recovery process obtains appropriate magnesium hydroxide impurity and purification, filtration finally obtain pure
Two aqueous magnesium chloride clarified solutions；Calcium chloride and manganese chloride generate hydroxide precipitation scrubbed drying, drying and crushing, classification respectively
Screening, packaging respectively obtain calcium hydroxide and manganous hydroxide product；The clarification magnesium chloride obtained with dibastic sodium phosphate based on pure material
Mass ratio 1: 1.61～2.04 react in the second corrosion-resistant reactor；Under agitation generate seven water magnesium monohydrogen phosphate and sodium chloride
Mixed solution；It is filtrated to get the scrubbed drying of filter cake, drying and crushing, is packaged to be seven water magnesium monohydrogen phosphate products；Continue heating dry
Dry bake out four crystalline water molecules and obtain three water magnesium monohydrogen phosphate products；The clear filtrate obtained is sent into decompression distiller and carries out decompression steaming
Evaporating, being ejected by distillate when solution reaches saturated concentration time cooled has a crystallization, scrubbed, dry, pulverize and obtain
Sodium chloride crystal product.
Boron mud the most according to claim 1 produces water-bearing phosphate hydrogen magnesium co-producing calcium hydroxide and the method for sodium chloride, and it is special
Levy and be: described boron mud, containing magnesia, silica, carbon dioxide, boron oxide, calcium oxide, manganese oxide in its component
And moisture content.
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| CN201410478054.9A CN105883744A (en) | 2014-09-12 | 2014-09-12 | Method for co-production of hydrous magnesium hydrogen phosphate, calcium hydrate and sodium chloride from boron mud |
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| CN201410478054.9A CN105883744A (en) | 2014-09-12 | 2014-09-12 | Method for co-production of hydrous magnesium hydrogen phosphate, calcium hydrate and sodium chloride from boron mud |
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Cited By (1)
| 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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- 2014-09-12 CN CN201410478054.9A patent/CN105883744A/en active Pending
Cited By (1)
| 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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