CN109941969A - Utilize the method for disodium hydrogen phosphate processing waste sulfuric acid solution - Google Patents
Utilize the method for disodium hydrogen phosphate processing waste sulfuric acid solution Download PDFInfo
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- CN109941969A CN109941969A CN201910334066.7A CN201910334066A CN109941969A CN 109941969 A CN109941969 A CN 109941969A CN 201910334066 A CN201910334066 A CN 201910334066A CN 109941969 A CN109941969 A CN 109941969A
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- sulfuric acid
- acid solution
- disodium hydrogen
- hydrogen phosphate
- waste sulfuric
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Abstract
The invention belongs to waste acid liquor processing technology fields, and in particular to utilize the method for disodium hydrogen phosphate processing waste sulfuric acid solution.The technical problem to be solved by the present invention is to the method higher costs of existing processing waste sulfuric acid solution.The invention discloses the methods using disodium hydrogen phosphate processing waste sulfuric acid solution, include the following steps: disodium hydrogen phosphate and waste sulfuric acid solution is separated in same closed container at normal temperature, until the mass concentration of sulfuric acid is 50~55% in waste sulfuric acid solution, sulfuric acid solution and water-bearing phosphate disodium hydrogen after being handled.The concentration that waste sulfuric acid solution is improved using the method for the present invention efficiently utilizes useless raw material, and alleviates pressure caused by environment, and reduce costs.
Description
Technical field
The invention belongs to waste acid liquor processing technology fields, and in particular to utilize disodium hydrogen phosphate processing waste sulfuric acid solution
Method.
Background technique
Titanium dioxide is a kind of excellent white pigment, is widely used in paint, coating, papermaking, plastics and electric welding at present
The industries such as item.
Currently, the technique of production titanium dioxide mainly has sulfuric acid process and chloridising, two kinds of techniques are simultaneously deposited, and production capacity and yield
It is very huge.However, both production technologies all have certain environmental pressure.It is raw for Production By Sulfuric Acid Process technique
Green vitriol (FeSO during production by a large amount of hydrolysis spent acid is generated and containing seven crystallizations water4·7H2O).When with ilmenite concentrate
(main component is metatitanic acid iron FeTiO3, wherein the content of titanium dioxide is 45-50 weight %) and when being raw material, generally produce 1
3.5~4 ton of seven inkstone of output is generated 7~8 tons of hydrolysis spent acid for containing 20% sulfuric acid by ton titanium dioxide.
There is processing difficulty in view of a large amount of green vitriols in European countries, therefore turn to chloridising production to avoid.This
Outside, high titanium slag is used to carry out Production By Sulfuric Acid Process for raw material, though the problem of can avoid green vitriol, the utilization of hydrolysis Waste Sulfuric Acid is still
In the presence of.
Due to too big using the waste sulfuric acid solution quantum of output of method for producing gtitanium dioxide with sulphuric acid by-product, and contain a certain amount of sulphur
It is sour ferrous, so that this waste sulfuric acid solution can not be utilized in other fields using dilute sulfuric acid.Currently, generalling use lime
The method that stone carries out neutralizing generation calcium sulfate handles this waste sulfuric acid solution.However, obtained calcium sulfate does not utilize
It is worth and can only store up, not only utilize raw material well, but also biggish pressure can be caused to environment.
The prior art, which also first passes through evaporation, makes the concentration of waste sulfuric acid solution be increased to 30%~40%, isolates sulfuric acid Asia
Iron, further evaporation makes the concentration of waste sulfuric acid solution be increased to 50% or more, returns to acidolysis operation, uses for continuous acidolysis,
To be fully exploited.But corrosivity is extremely strong at high temperature for sulfuric acid solution, it is desirable that it is worth higher graphite material, meanwhile,
It is concentrated by evaporation the steam boiler for needing large capacity, so that the equipment investment of this method is high.
Summary of the invention
The technical problem to be solved by the present invention is to the method for existing processing waste sulfuric acid solution is at high cost.
The technical solution used to solve the technical problems of the present invention is that providing molten using disodium hydrogen phosphate processing Waste Sulfuric Acid
The method of liquid.Include the following steps: disodium hydrogen phosphate and waste sulfuric acid solution is separated in same closed container at normal temperature
In, until the mass concentration of sulfuric acid is 50~55% in waste sulfuric acid solution, sulfuric acid solution and water-bearing phosphate hydrogen two after being handled
Sodium.
Wherein, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, every 100 weight of waste sulfuric acid solution
Part is measured, 40~85 parts by weight of disodium hydrogen phosphate are used.
Further, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, the waste sulfuric acid solution is every
100 parts by weight use 80~85 parts by weight of disodium hydrogen phosphate.
Further, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, the time of the placement is
Half cycle~1 week.
Wherein, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, the waste sulfuric acid solution is by sulphur
Acid system prepares the by-product of titanium dioxide generation.
Further, sulfuric acid and ferrous sulfate are contained in the waste sulfuric acid solution, using the total weight of waste sulfuric acid solution as base
Standard, the concentration of sulfuric acid is not higher than 20% in the waste sulfuric acid solution.
Further, the concentration of sulfuric acid is 17~20% in the waste sulfuric acid solution, and the concentration of ferrous sulfate is 2~3%.
Wherein, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, the water-bearing phosphate disodium hydrogen exists
95~100 DEG C are dried to obtain disodium hydrogen phosphate, and disodium hydrogen phosphate continues to use processing waste sulfuric acid solution.
Further, the water-bearing phosphate disodium hydrogen includes six water disodium hydrogen phosphates and disodium hydrogen phosphate.
Wherein, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, sulfuric acid solution is used after the processing
In dissolution ilmenite concentrate to prepare titanium dioxide.
Wherein, in the above-mentioned method using disodium hydrogen phosphate processing waste sulfuric acid solution, when gained water-bearing phosphate disodium hydrogen
It is when the saturation state that not up to absorbs water, water-bearing phosphate disodium hydrogen and new waste sulfuric acid solution is separated in same closed container
In, until being completely reformed into disodium hydrogen phosphate, takes out disodium hydrogen phosphate and be dried, be recycled；It is closed
Remaining waste sulfuric acid solution continues to place with the disodium hydrogen phosphate not absorbed water in container, until sulfuric acid concentration reaches 50% or more,
The hydrolysis procedure for returning to sulfate process titanium dioxide uses.
The beneficial effects of the present invention are:
The method of the present invention completely avoids the use of boiler and evaporator, avoids the use of expensive resistant material,
To reduce fixed investment, and operation carries out under conditions of room temperature, significantly improves operating condition in this way, but also
The economy of Waste Sulfuric Acid concentration is improved.Waste acid treatment method provided by the invention not only efficiently utilizes Producing Titanium Dioxide institute
The scrap feed material of generation, but also can reduce the pressure caused by environment, improves operating environment, before great industrial application
Scape.
Specific embodiment
Waste sulfuric acid solution is handled using existing method, cannot not only efficiently use raw material, but also environment can be given
Cause biggish pressure.Although using positive evaporating concentrating method, can by waste sulfuric acid solution return acidolysis carry out using,
It is that sulfuric acid solution corrosivity is high during high temperature evaporation, it is desirable that evaporation equipment has high corrosion resistance, and evaporation is set
Standby price general charged is higher, causes the processing cost of waste sulfuric acid solution to improve, also, the service life of evaporation equipment is shorter.Therefore,
After study, can handle to obtain using the equipment that technical solution of the present invention does not need valuableness can return to acidolysis use to inventor
Sulfuric acid solution.
Specifically, the present invention provides the methods using disodium hydrogen phosphate processing waste sulfuric acid solution.Including the following steps: will
Disodium hydrogen phosphate and waste sulfuric acid solution are separated in same closed container at normal temperature, until sulfuric acid in waste sulfuric acid solution
Mass concentration is 50~55%, sulfuric acid solution and water-bearing phosphate disodium hydrogen after being handled.
The concentration of sulfuric acid is 17~20% in the waste sulfuric acid solution that the present invention uses, and the concentration of ferrous sulfate is 2~3%.
In the present invention, every 100 parts by weight of the waste sulfuric acid solution used, use 40~85 parts by weight of disodium hydrogen phosphate.Phosphorus
The dosage of sour disodium hydrogen and the time of concentration are to be mutually related, and the dosage of disodium hydrogen phosphate is more, then concentration time is short, phosphoric acid hydrogen
The dosage of disodium is few, then concentration time is long, and in order to make concentration time reduce one times, every 100 parts by weight of waste sulfuric acid solution be can be used
80~85 parts by weight of disodium hydrogen phosphate.
In the past to the processing of Waste Sulfuric Acid, it is exactly to be stored up in lime with generation calcium sulfate, due to having spent acid, pollutes ring
Border.As environmental protection policy is increasingly stringent, handled using being concentrated by evaporation, and the corrosivity of sulfuric acid at relatively high temperatures is extremely strong, one
As will using graphite plate, pipe, add steam boiler etc., invest high maintenance costs it is also larger.Therefore, the economy of the method for the present invention
Clearly.
The solution of the present invention is explained below in conjunction with embodiment.It will be understood to those of skill in the art that following
Embodiment is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Particular technique or item are not specified in embodiment
Part, it described technology or conditions or is carried out according to the literature in the art according to product description.Agents useful for same or instrument
Production firm person is not specified in device, and being can be with conventional products that are commercially available.
The present invention will further be elaborated by specific embodiment below.
In the present invention, concentration is mass percent.
Embodiment 1
The sulfuric acid for being 20% containing concentration by 100g, the waste sulfuric acid solution and 40g disodium hydrogen phosphate of 2~3% ferrous sulfate
The separated sulfuric acid solution and ten hydrogen phosphate dihydrates two for obtaining concentration after 1 week in same closed container and being 50% at normal temperature
Sodium uses in the step of 50% sulfuric acid solution is returned to method for producing gtitanium dioxide with sulphuric acid, by disodium hydrogen phosphate 95~
100 DEG C are dried the removing crystallization water, continue on for handling waste sulfuric acid solution.
Embodiment 2
The sulfuric acid for being 20% containing concentration by 100g, the waste sulfuric acid solution and 80g disodium hydrogen phosphate of 2~3% ferrous sulfate
The separated sulfuric acid solution and six water disodium hydrogen phosphates for obtaining concentration after 3.5 days in closed container and being 50% at normal temperature,
It is used in the step of 50% sulfuric acid solution is returned to method for producing gtitanium dioxide with sulphuric acid, by six water disodium hydrogen phosphates at 95~100 DEG C
The removing crystallization water is dried, continues on for handling waste sulfuric acid solution.
Embodiment 3
In order to improve the utilization rate of disodium hydrogen phosphate, the mode of operation of " adverse current " can be used.
The sulfuric acid that the six water disodium hydrogen phosphates and 100g that embodiment 2 is obtained are 20% containing concentration, 2~3% sulfuric acid are sub-
The waste sulfuric acid solution of iron is separated in same closed container at normal temperature, and the sulfuric acid solution that concentration is 50% is obtained after 1 week
And disodium hydrogen phosphate, the removing crystallization water is dried at 95~100 DEG C in disodium hydrogen phosphate, obtains phosphoric acid hydrogen
Disodium continues on for handling waste sulfuric acid solution.
The sulfuric acid solution that concentration is 50% continues, half cycle separated in closed container at normal temperature with disodium hydrogen phosphate
It is used in the step of obtaining the sulfuric acid solution that concentration is 55% afterwards, returning to method for producing gtitanium dioxide with sulphuric acid.
Solid phase disodium hydrogen phosphate still has the space of water suction, its continuation is allowed to separate in closed container with new waste sulfuric acid solution
It places, until disodium hydrogen phosphate saturation is disodium hydrogen phosphate, disodium hydrogen phosphate is dry de- at 95~100 DEG C
Continue on for handling waste sulfuric acid solution except the crystallization water obtains disodium hydrogen phosphate.Waste sulfuric acid solution is continued and new disodium hydrogen phosphate
Effect, until sulfuric acid concentration reaches 55% and stops.
Claims (7)
1. utilizing the method for disodium hydrogen phosphate processing waste sulfuric acid solution, characterized by the following steps: by disodium hydrogen phosphate
It is separated in same closed container at normal temperature with waste sulfuric acid solution, until the mass concentration of sulfuric acid is in waste sulfuric acid solution
50~55%, sulfuric acid solution and water-bearing phosphate disodium hydrogen after being handled.
2. the method according to claim 1 using disodium hydrogen phosphate processing waste sulfuric acid solution, it is characterised in that: described useless
Every 100 parts by weight of sulfuric acid solution, use 40~85 parts by weight of disodium hydrogen phosphate.
3. the method according to claim 2 using disodium hydrogen phosphate processing waste sulfuric acid solution, it is characterised in that: described useless
Every 100 parts by weight of sulfuric acid solution, use 80~85 parts by weight of disodium hydrogen phosphate.
4. the method according to claim 1 using disodium hydrogen phosphate processing waste sulfuric acid solution, it is characterised in that: described useless
Sulfuric acid solution is the by-product generated by method for producing gtitanium dioxide with sulphuric acid.
5. the method according to claim 1 using disodium hydrogen phosphate processing waste sulfuric acid solution, it is characterised in that: described to contain
Water disodium hydrogen phosphate is dried to obtain disodium hydrogen phosphate at 95~100 DEG C, and disodium hydrogen phosphate continues to use processing waste sulfuric acid solution.
6. described in any item methods using disodium hydrogen phosphate processing waste sulfuric acid solution, feature exist according to claim 1~5
In: sulfuric acid solution is for dissolving ilmenite concentrate to prepare titanium dioxide after the processing.
7. the method according to claim 1 using disodium hydrogen phosphate processing waste sulfuric acid solution, it is characterised in that: work as gained
Water-bearing phosphate disodium hydrogen not up to absorb water saturation state when, by water-bearing phosphate disodium hydrogen and new waste sulfuric acid solution it is separated in
In same closed container, until being completely reformed into disodium hydrogen phosphate, takes out disodium hydrogen phosphate and be dried, follow
Ring uses；Remaining waste sulfuric acid solution continues to place with the disodium hydrogen phosphate not absorbed water in closed container, until sulfuric acid concentration reaches
To 50% or more, the hydrolysis procedure for returning to sulfate process titanium dioxide is used.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525187A (en) * | 2009-03-24 | 2009-09-09 | 四川大学 | Method for concentrating titanium pigment waste acid |
| CN101538023A (en) * | 2008-03-22 | 2009-09-23 | 四川大学 | Processing method for titanium pigment waste acid |
| CN102910594A (en) * | 2012-11-06 | 2013-02-06 | 黄正源 | Method for concentrating waste sulfuric acid by utilizing waste heat of titanium dioxide calcinator |
-
2019
- 2019-04-24 CN CN201910334066.7A patent/CN109941969A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538023A (en) * | 2008-03-22 | 2009-09-23 | 四川大学 | Processing method for titanium pigment waste acid |
| CN101525187A (en) * | 2009-03-24 | 2009-09-09 | 四川大学 | Method for concentrating titanium pigment waste acid |
| CN102910594A (en) * | 2012-11-06 | 2013-02-06 | 黄正源 | Method for concentrating waste sulfuric acid by utilizing waste heat of titanium dioxide calcinator |
Non-Patent Citations (1)
| Title |
|---|
| 朱洪法 等: "《无机化工产品手册》", 31 December 2008, 金盾出版社 * |
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