CN106745114A - A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium - Google Patents

A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium Download PDF

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Publication number
CN106745114A
CN106745114A CN201611092701.8A CN201611092701A CN106745114A CN 106745114 A CN106745114 A CN 106745114A CN 201611092701 A CN201611092701 A CN 201611092701A CN 106745114 A CN106745114 A CN 106745114A
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CN
China
Prior art keywords
sulfuric acid
waste sulfuric
alkylation
residue
waste
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Pending
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CN201611092701.8A
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Chinese (zh)
Inventor
岑忠儒
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Fangchenggang Wuxing Chemical Co Ltd
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Fangchenggang Wuxing Chemical Co Ltd
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Priority to CN201611092701.8A priority Critical patent/CN106745114A/en
Publication of CN106745114A publication Critical patent/CN106745114A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/40Magnesium sulfates
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05DINORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D3/00Calcareous fertilisers
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05DINORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D5/00Fertilisers containing magnesium

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Fertilizers (AREA)

Abstract

The present invention relates to a kind for the treatment of of Waste Sulfuric Acid, especially a kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium, comprises the steps of:(1) waste sulfuric acid from alkylation is added to and 90 DEG C is preheating in reactor;(2) magnesite powder is added while stirring, is produced to bubble-free;(3) it is 6.8~7.0 to add light-burning magnesium powder to be reacted to ph, obtains mixed liquor;(4) by the isolated mother liquor of above-mentioned mixed liquor press filtration and a waste residue;(5) SODIUM PERCARBONATE is added in a mother liquor and is stirred;(6) press filtration obtains secondary mother liquid and secondary residue;(7) secondary mother liquid is obtained epsom salt by crystallization, centrifugation, drying;(8) waste residue and secondary residue are well mixed, are crushed after drying and silico-calcium kieserite is obtained.A kind of utilization waste sulfuric acid from alkylation production magnesium sulfate and method process is simple, low cost, the non-secondary pollution of fertiliser containing magnesium that the present invention is provided.

Description

A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium
Technical field
It is especially a kind of to produce magnesium sulfate and fertiliser containing magnesium using waste sulfuric acid from alkylation the present invention relates to a kind for the treatment of of Waste Sulfuric Acid Method.
Background technology
Raw material magnesia used in waste sulfuric acid from alkylation production magnesium sulfate is removed and contains 85%~90% available oxidation Outside magnesium, also containing about 10~15% insoluble matter, its Main Ingredients and Appearance is silica and calcium oxide, and these insoluble matters are anti-through sulfuric acid Finally it is brought into residue after answering.Therefore, the main component of residue is:Magnesium sulfate that silica, calcium sulfate, mother liquor bring, The components such as string, activated carbon of sorbent that catalyst brings.
It is domestic at present commonplace using siliceous fertilizer, calcium silicate fertilizer, silicon-calcium-magnesium fertilizer, kieserite etc., it is used mostly various containing Silicon waste slag is produced, and typically all particle is hard, indissoluble solution, fertilizer efficiency are relatively low.Magnesia residue contains abundant silicon, calcium, magnesium, sulphur, The small activity of particle is high, but does not produce the technology of silico-calcium kieserite using magnesia waste residue still.
The content of the invention
To solve the above problems, the present invention provides a kind of low cost, one kind of non-secondary pollution and utilizes waste sulfuric acid from alkylation The method of production magnesium sulfate and fertiliser containing magnesium, concrete technical scheme is:
A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and silico-calcium kieserite, comprises the steps of:
(1) waste sulfuric acid from alkylation is added to and 90 DEG C is preheating in reactor;
(2) magnesite powder is added while stirring, is produced to bubble-free;
(3) it is 6.8~7.0 to add light-burning magnesium powder to be reacted to ph, obtains mixed liquor;
(4) by the isolated mother liquor of above-mentioned mixed liquor press filtration and a waste residue;
(5) SODIUM PERCARBONATE is added in a mother liquor and is stirred;
(6) press filtration obtains secondary mother liquid and secondary residue;
(7) secondary mother liquid is obtained epsom salt by crystallization, centrifugation, drying;
(8) waste residue and secondary residue are well mixed, are crushed after drying and silico-calcium kieserite is obtained.
Waste sulfuric acid from alkylation described in step 1 is the Waste Sulfuric Acid of the alkylated reaction by-product that catalyst is made using sulfuric acid, is given up Sulfuric acid concentration is 75~86wt%.
The quality of the sodium carbonate described in step 5 is the 6~10% of Waste Sulfuric Acid quality.
The method consumes sulfuric acid by producing magnesium sulfate, and acid-soluble oil is gone out using the suspension adsorbing separation such as silicon, calcium in miberal powder Waste residue, production mainly contains the fertilizer of silicon-calcium-magnesium sulphur.
A kind of utilization waste sulfuric acid from alkylation production magnesium sulfate and method process is simple, the cost of fertiliser containing magnesium that the present invention is provided Low, non-secondary pollution.
Specific embodiment
It is described further by the following examples.
Embodiment one
A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and silico-calcium kieserite, comprises the steps of:
(1) 500kg waste sulfuric acid from alkylation is added to and 90 DEG C is preheating in reactor, sulfur waste acid concentration is 78wt%;
(2) 500kg magnesite powders are added while stirring, are produced to bubble-free;
(3) it is 6.9 to add 400kg light-burning magnesium powders to be reacted to ph, obtains mixed liquor;
(4) by the isolated mother liquor of above-mentioned mixed liquor press filtration and a waste residue;
(5) 50kg sodium carbonate was added in a mother liquor and was stirred;
(6) press filtration obtains secondary mother liquid and secondary residue;
(7) secondary mother liquid is obtained epsom salt by crystallization, centrifugation, drying;
(8) waste residue and secondary residue are well mixed, are crushed after drying and silico-calcium kieserite is obtained.
Embodiment two
A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and silico-calcium kieserite, comprises the steps of:
(1) 100kg waste sulfuric acid from alkylation is added to and 90 DEG C is preheating in reactor, sulfur waste acid concentration is 76wt%;
(2) 120kg magnesite powders are added while stirring, are produced to bubble-free;
(3) it is 7.0 to add 80 this light-burning magnesium powder to be reacted to ph, obtains mixed liquor;
(4) by the isolated mother liquor of above-mentioned mixed liquor press filtration and a waste residue;
(5) 6kg SODIUM PERCARBONATEs are added in a mother liquor and is stirred;
(6) press filtration obtains secondary mother liquid and secondary residue;
(7) secondary mother liquid is obtained epsom salt by crystallization, centrifugation, drying;
(8) waste residue and secondary residue are well mixed, are crushed after drying and silico-calcium kieserite is obtained.

Claims (3)

1. a kind of method that utilization waste sulfuric acid from alkylation produces magnesium sulfate and silico-calcium kieserite, it is characterised in that comprising following step Suddenly:
(1) waste sulfuric acid from alkylation is added to and 90 DEG C is preheating in reactor;
(2) magnesite powder is added while stirring, is produced to bubble-free;
(3) it is 6.8~7.0 to add light-burning magnesium powder to be reacted to ph, obtains mixed liquor;
(4) by the isolated mother liquor of above-mentioned mixed liquor press filtration and a waste residue;
(5) SODIUM PERCARBONATE is added in a mother liquor and is stirred;
(6) press filtration obtains secondary mother liquid and secondary residue;
(7) secondary mother liquid is obtained epsom salt by crystallization, centrifugation, drying;
(8) waste residue and secondary residue are well mixed, are crushed after drying and silico-calcium kieserite is obtained.
2. the method that a kind of utilization waste sulfuric acid from alkylation according to claim 1 produces magnesium sulfate and fertiliser containing magnesium, its feature exists In waste sulfuric acid from alkylation described in step 1 is the Waste Sulfuric Acid of the alkylated reaction by-product that catalyst is made using sulfuric acid, and Waste Sulfuric Acid is dense It is 75~86wt% to spend.
3. the method that a kind of utilization waste sulfuric acid from alkylation according to claim 1 produces magnesium sulfate and fertiliser containing magnesium, its feature exists In the quality of sodium carbonate described in step 5 is the 6~10% of Waste Sulfuric Acid quality.
CN201611092701.8A 2016-12-01 2016-12-01 A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium Pending CN106745114A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611092701.8A CN106745114A (en) 2016-12-01 2016-12-01 A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611092701.8A CN106745114A (en) 2016-12-01 2016-12-01 A kind of method of utilization waste sulfuric acid from alkylation production magnesium sulfate and fertiliser containing magnesium

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CN106745114A true CN106745114A (en) 2017-05-31

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112429754A (en) * 2020-11-15 2021-03-02 盘锦泓实环保科技有限公司 Large-particle magnesium sulfate cooling crystallization method and system
BE1030582B1 (en) * 2022-06-02 2024-01-08 Univ Tianjin Technology METHOD FOR PRODUCING MAGNESIUM SILICON SULFATE-CALCIUM-SULFUR-MAGNESIUM FERTILIZER FROM SPENT SULFURIC ACID PRODUCED DURING ALKYLATION

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112429754A (en) * 2020-11-15 2021-03-02 盘锦泓实环保科技有限公司 Large-particle magnesium sulfate cooling crystallization method and system
BE1030582B1 (en) * 2022-06-02 2024-01-08 Univ Tianjin Technology METHOD FOR PRODUCING MAGNESIUM SILICON SULFATE-CALCIUM-SULFUR-MAGNESIUM FERTILIZER FROM SPENT SULFURIC ACID PRODUCED DURING ALKYLATION

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