CN109837592B - A kind of joint disposal of industrial wastes utilizes method - Google Patents
A kind of joint disposal of industrial wastes utilizes method Download PDFInfo
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- CN109837592B CN109837592B CN201910173097.9A CN201910173097A CN109837592B CN 109837592 B CN109837592 B CN 109837592B CN 201910173097 A CN201910173097 A CN 201910173097A CN 109837592 B CN109837592 B CN 109837592B
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Abstract
The present invention relates to a kind of joint disposals of industrial wastes to utilize method, comprises the following steps: 1) crushing shell, adds hydrochloride waste, stirs, obtains reaction solution A；2) reaction solution A is filtered, and obtains filtrate；3) filtrate is heated, sanlose, sodium tripolyphosphate and chelating agent is added, then sulfuric acid waste is at the uniform velocity added dropwise, obtains reaction solution B；4) reaction solution B is filtered, and filter cake is cleaned with hot water, is dried under reduced pressure, and obtains calcium sulfate crystal whiskers.The present invention, which realizes industrial wastes, to turn waste into wealth, and decreases the environmental pollution of industrial wastes.
Description
Technical field
The present invention relates to a kind of joint disposals of industrial wastes to utilize method.
Background technique
From 1996, China was sure to occupy the status of the first in the world steel big producer for years, with building, machine
The development of tool, light industry person's electrical domain, China's steel industry production scale is yet in continuous enlargement.Pickling is clean metal surface one
Kind method and the necessary process of steel production and processing, the purpose is to remove the oxide of metal surface.In acid cleaning process,
Acid cleaner is contacted and is reacted with metal surface, with the increasing of the reduction of ammonia ion concentration and concentration of metal ions in acid
Add, the pickling efficiency of acid solution also constantly reduces, and becomes the pickle liquor for needing outlet.Currently, main in acid washing rolled steel technique
Acid cleaner has hydrochloric acid, sulfuric acid and nitric acid etc., and wherein nitric acid is mainly used for the surface clean of Stainless Steel.For common iron, salt
The pickling effect of acid is more significant compared with sulfuric acid, and the release effect of chlorohydric acid pickling keeps base iron loss less, and hydrochloric acid is increasingly becoming
Mainstream cleaning agent in steel cleaning process.
Contain a large amount of H in acid washing rolled steel waste liquid+And Fe2+Based on metal ion, if direct emission will seriously affect water
The ecological environment of body and soil poisons surrounding animals and plants, causes soil property calcification, destroys soil layer construction；If people and animals accidentally drink acidity compared with
Big water gently then causes stomach salt, heavy then digestive system of burning；If taking in excessive heavy metal ion, people and animals' metal also will cause
Poisoning, finally causes to seriously endanger to human health.In addition to this, pickle liquor is because of its acidity height, to biological wastewater treatment system
Biological self reproducing in system also has certain influence, can also endanger the water conservancy project structures such as sewer pipe and armored concrete, cause burn into
Destroy etc..Meanwhile pickle liquor acidity is high, molysite content is big, if direct emission is also a kind of waste of resource.
Environment is not only polluted in the discharge of pickle liquor, and changing in resource and economically is a kind of waste.Acid and gold in spent acid
Category can be transferred through reasonable recycling mode recycling and reusing, in addition to produce byproduct, regenerated acid can direct reuse in pickling work
Skill not only reduces production cost, can also increase economic benefit.Therefore, to spent acid and again with suitable resource treatment technique
Metal ion, which is recycled, to be particularly important.
Calcium sulfate crystal whiskers are CaSO4Fibrous monocrystal has calcium sulphate dihydrate, half-H 2 O calcium sulphate and anhydrous calcium sulfate whisker
Three kinds of point, wherein anhydrous calcium sulfate whisker use value and economic value highest, the most commonly used.Calcium sulfate crystal whiskers are as enhancing
Materials'use has dimensionally stable, intensity height, good toughness, corrosion-and high-temp-resistant, is easy to many excellent physics and chemistry such as surface treatment
Performance has a wide range of applications, and if calcium sulfate crystal whiskers are used as the filler of moderate strength, calcium sulfate crystal whiskers are mentioned for plastic products
Tensile strength, bending strength, elasticity modulus and heat distortion temperature of high product etc..Calcium Sulfate Whiskers are smaller, whisker is longer,
Performance is better.
Chinese patent CN201010514539.0 discloses a kind of utilization solvay liquor and Waste Sulfuric Acid high-quality calcium sulfate
The method of whisker, is that 50~90% Waste Sulfuric Acids are heated to be 40~140 DEG C for mass content, then by the solvay liquor chlorination after preheating
Calcium solution is gradually added in Waste Sulfuric Acid, heating and thermal insulation in reaction process, obtains that surface is smooth, diameter is small, the big calcium sulfate of draw ratio
Whisker.But there are apparent defect and deficiencies for above-mentioned calcium sulphate crystal whisker preparation method: (1) reaction process is needed using special
Heating method carry out heating and thermal insulation, with guarantee heating process even heat stablize, the process is to temperature control requirement height；(2)
In order to reach the accurate temperature control of reaction process, solvay liquor calcium chloride solution need to preheat in advance, and need to be consistent with Waste Sulfuric Acid temperature.
Chinese patent 201610778544.X discloses the joint disposal of sulfuric acid waste and hydrochloride waste a kind of using method,
Calcium sulfate crystal whiskers are prepared using sulfuric acid waste, hydrochloride waste and shell, preparation method comprises the following steps: shell is crushed, then
Hydrochloride waste is added, stirring reacts 1~2h, obtains reaction solution A；Filtrate is heated to 70~90 DEG C after reaction solution A filtering, is added
Enter sanlose, sodium tripolyphosphate and chelating agent I, then sulfuric acid waste is at the uniform velocity added dropwise, reacts 1~2h, reacted
Liquid B；Reaction solution B filtering, filter cake is cleaned with 60~80 DEG C of hot water, then is dried under reduced pressure 2h at 110~130 DEG C.Reduce sulfuric acid
The production cost of calcium pyroborate, prepared Calcium Sulfate Whiskers are small, whisker is long, and are evenly distributed.But above-mentioned calcium sulfate is brilliant
There are apparent defect and deficiencies for palpus preparation method: Calcium Sulfate Whiskers are still bigger than normal, and whisker length is still partially short, finally lead
Cause draw ratio still relatively low, prepared calcium sulfate crystal whiskers can not high-grade plastic products needs, can not also increase substantially anti-
Tensile strength, bending strength, elasticity modulus and heat distortion temperature etc..
Therefore, how high added value is located in reason industrial wastes and is prepared that diameter is smaller, whisker is longer, long using industrial wastes
Diameter becomes this field technical issues that need to address than higher calcium sulfate crystal whiskers.
Summary of the invention
In order to solve in the prior art, how high added value is located in reason industrial wastes and prepares diameter more using industrial wastes
It is small, whisker is longer, the higher calcium sulfate crystal whiskers of draw ratio, the invention proposes following technical solutions:
A kind of joint disposal of industrial wastes utilizes method, and the industrial wastes includes hydrochloride waste and sulfuric acid waste, institute
Joint disposal is stated to comprise the following steps using method:
1) shell is crushed, adds hydrochloride waste, the molar ratio of hydrochloric acid and calcium carbonate in shell in the hydrochloride waste
For 2~2.2:1, stirring reacts 1~2h, obtains reaction solution A；
2) reaction solution A is filtered, and obtains filtrate；
3) filtrate is heated to 80 DEG C, sanlose, sodium tripolyphosphate and chelating agent I is added, then at the uniform velocity drip
Add sulfuric acid waste, reacts 1~2h, obtain reaction solution B, the molar ratio of sulfuric acid and calcium carbonate in shell is in the sulfuric acid waste
0.9~1:1；
4) reaction solution B is filtered, and filter cake is cleaned with 80 DEG C of hot water, then is dried under reduced pressure 2h at 120 DEG C, obtains calcium sulfate crystalline substance
Palpus；
The chelating agent I has following structural formula:
Preferably, the weight of the step 3) sanlose is the 15~20% of shell weight.
Preferably, the weight of the step 3) sodium tripolyphosphate is the 0.3~0.5% of shell weight.
Preferably, the weight of step 3) the chelating agent I is the 0.3~0.5% of shell weight.
Preferably, the time for adding of the step 3) sulfuric acid waste is 20min.
Technical solution of the present invention has as follows by beneficial effect:
(1) realizing hydrochloride waste and sulfuric acid waste turns waste into wealth, and greatly reduces the production cost of calcium sulfate crystal whiskers,
Reduce the environmental pollution of hydrochloride waste and sulfuric acid waste.
(2) the above results show that the present invention using sanlose, increases the viscosity of reaction system, slows down sulphur
The sinking speed of sour calcium pyroborate, effect are much better than used glycerol in the prior art.Further, the present invention uses trimerization
The growth of sodium phosphate and chelating agent I regulation calcium sulfate crystal whiskers, chelate effect are much better than used hydroxide in the prior art
Magnesium and ethylenediamine tetra-acetic acid.Further, the present invention utilizes between sanlose, sodium tripolyphosphate and chelating agent I
Synergistic effect regulation calcium sulfate crystal whiskers diameter and whisker length, the diameter of prepared calcium sulfate crystal whiskers is small, whisker is long, and
It is evenly distributed, improves the purity and performance of anhydrous calcium sulfate whisker.The present invention successfully solves existing anhydrous calcium sulfate whisker
Preparation disadvantage, i.e., (1) although prepared by the smaller whisker of Calcium Sulfate Whiskers it is very short, or sulfuric acid prepared by (2)
Although calcium pyroborate is longer but diameter is very big, also exactly above-mentioned two o'clock disadvantage limits the application of calcium sulfate crystal whiskers.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments and comparative example,
The present invention will be described in further detail.
Embodiment 1
A kind of joint disposal of industrial wastes utilizes method, and the industrial wastes includes hydrochloride waste and sulfuric acid waste, institute
Joint disposal is stated to comprise the following steps using method:
1) shell is crushed, adds hydrochloride waste, the molar ratio of hydrochloric acid and calcium carbonate in shell in the hydrochloride waste
For 2:1, stirring reacts 1h, obtains reaction solution A；
2) reaction solution A is filtered, and obtains filtrate；
3) filtrate is heated to 80 DEG C, sanlose, sodium tripolyphosphate and chelating agent I is added, then at the uniform velocity drip
Add sulfuric acid waste, react 1h, obtain reaction solution B, the molar ratio of sulfuric acid and calcium carbonate in shell is 0.9 in the sulfuric acid waste:
1；
4) reaction solution B is filtered, and filter cake is cleaned with 80 DEG C of hot water, then is dried under reduced pressure 2h at 120 DEG C, obtains calcium sulfate crystalline substance
Palpus；
The chelating agent I has following structural formula:
The weight of the step 3) sanlose is the 15% of shell weight.
The weight of the step 3) sodium tripolyphosphate is the 0.3% of shell weight.
The weight of step 3) the chelating agent I is the 0.3% of shell weight.
The time for adding of the step 3) sulfuric acid waste is 20min.
Embodiment 2
A kind of joint disposal of industrial wastes utilizes method, and the industrial wastes includes hydrochloride waste and sulfuric acid waste, institute
Joint disposal is stated to comprise the following steps using method:
1) shell is crushed, adds hydrochloride waste, the molar ratio of hydrochloric acid and calcium carbonate in shell in the hydrochloride waste
For 2.1:1, stirring reacts 1.5h, obtains reaction solution A；
2) reaction solution A is filtered, and obtains filtrate；
3) filtrate is heated to 80 DEG C, sanlose, sodium tripolyphosphate and chelating agent I is added, then at the uniform velocity drip
Add sulfuric acid waste, react 1.5h, obtain reaction solution B, the molar ratio of sulfuric acid and calcium carbonate in shell is 1 in the sulfuric acid waste:
1；
4) reaction solution B is filtered, and filter cake is cleaned with 80 DEG C of hot water, then is dried under reduced pressure 2h at 120 DEG C, obtains calcium sulfate crystalline substance
Palpus；
The chelating agent I has following structural formula:
The weight of the step 3) sanlose is the 18% of shell weight.
The weight of the step 3) sodium tripolyphosphate is the 0.4% of shell weight.
The weight of step 3) the chelating agent I is the 0.4% of shell weight.
The time for adding of the step 3) sulfuric acid waste is 20min.
Embodiment 3
A kind of joint disposal of industrial wastes utilizes method, and the industrial wastes includes hydrochloride waste and sulfuric acid waste, institute
Joint disposal is stated to comprise the following steps using method:
1) shell is crushed, adds hydrochloride waste, the molar ratio of hydrochloric acid and calcium carbonate in shell in the hydrochloride waste
For 2.2:1, stirring reacts 2h, obtains reaction solution A；
2) reaction solution A is filtered, and obtains filtrate；
3) filtrate is heated to 80 DEG C, sanlose, sodium tripolyphosphate and chelating agent I is added, then at the uniform velocity drip
Add sulfuric acid waste, react 2h, obtain reaction solution B, the molar ratio of sulfuric acid and calcium carbonate in shell is 1:1 in the sulfuric acid waste；
4) reaction solution B is filtered, and filter cake is cleaned with 80 DEG C of hot water, then is dried under reduced pressure 2h at 120 DEG C, obtains calcium sulfate crystalline substance
Palpus；
The chelating agent I has following structural formula:
The weight of the step 3) sanlose is the 20% of shell weight.
The weight of the step 3) sodium tripolyphosphate is the 0.5% of shell weight.
The weight of step 3) the chelating agent I is the 0.5% of shell weight.
The time for adding of the step 3) sulfuric acid waste is 20min.
Comparative example 1
Sanlose in embodiment 1 is replaced with glycerol, other contents and the complete phase of embodiment 1 by comparative example 1
Together.
Comparative example 2
Sodium tripolyphosphate in embodiment 1 and chelating agent I are replaced with magnesium hydroxide and ethylenediamine tetra-acetic acid by comparative example 2,
Its content is identical with embodiment 1.
Comparative example 3
Sanlose in embodiment 1 is replaced with glycerol by comparative example 3, and by sodium tripolyphosphate in embodiment 1
Magnesium hydroxide and ethylenediamine tetra-acetic acid are replaced with chelating agent I, other contents are identical with embodiment 1.
In order to verify the effect of embodiment 1-3 and comparative example 1-3, by measurement, 1-3 of the embodiment of the present invention and comparison are obtained
The average diameter and average whisker length of calcium sulfate crystal whiskers prepared by example 1-3 are as a result as follows:
| Number | Average diameter (μm) | Average whisker length (μm) |
| Embodiment 1 | 1.4 | 245 |
| Embodiment 2 | 1.3 | 255 |
| Embodiment 3 | 1.3 | 260 |
| Comparative example 1 | 1.6 | 200 |
| Comparative example 2 | 1.5 | 180 |
| Comparative example 3 | 1.7 | 160 |
The above results show that the present invention using sanlose, increases the viscosity of reaction system, slows down calcium sulfate
The sinking speed of whisker, effect are much better than used glycerol in the prior art.Further, the present invention uses tripolyphosphate
Sodium and chelating agent I regulation calcium sulfate crystal whiskers growth, chelate effect be much better than in the prior art used in magnesium hydroxide and
Ethylenediamine tetra-acetic acid.Further, the present invention utilizes the association between sanlose, sodium tripolyphosphate and chelating agent I
Same-action regulates and controls the diameter and whisker length of calcium sulfate crystal whiskers, and the diameter of prepared calcium sulfate crystal whiskers is small, whisker is long, and is distributed
Uniformly, the purity and performance of anhydrous calcium sulfate whisker are improved.The present invention successfully solves the system of existing anhydrous calcium sulfate whisker
Standby disadvantage, i.e. (1) although prepared by the smaller whisker of Calcium Sulfate Whiskers it is very short, or calcium sulfate prepared by (2) is brilliant
Although the longer but diameter of palpus is very big, also exactly above-mentioned two o'clock disadvantage limits the application of calcium sulfate crystal whiskers.
Claims (2)
1. a kind of joint disposal of industrial wastes utilizes method, which is characterized in that the industrial wastes includes hydrochloride waste and sulphur
Acid waste liquid, the joint disposal are comprised the following steps using method:
1) shell is crushed, adds hydrochloride waste, in the hydrochloride waste in hydrochloric acid and shell the molar ratio of calcium carbonate be 2~
2.2:1, stirring react 1~2h, obtain reaction solution A；
2) reaction solution A is filtered, and obtains filtrate；
3) filtrate is heated to 80 DEG C, sanlose, sodium tripolyphosphate and chelating agent I is added, then sulphur is at the uniform velocity added dropwise
Acid waste liquid reacts 1~2h, obtains reaction solution B, in the sulfuric acid waste in sulfuric acid and shell the molar ratio of calcium carbonate be 0.9~
1:1；
4) reaction solution B is filtered, and filter cake is cleaned with 80 DEG C of hot water, then is dried under reduced pressure 2h at 120 DEG C, obtains calcium sulfate crystal whiskers；
The chelating agent I has following structural formula:
；
The weight of the step 3) sanlose is the 15~20% of shell weight；
The weight of the step 3) sodium tripolyphosphate is the 0.3~0.5% of shell weight；
The weight of step 3) the chelating agent I is the 0.3~0.5% of shell weight.
2. the joint disposal of industrial wastes according to claim 1 utilizes method, which is characterized in that the step 3) sulfuric acid
The time for adding of waste liquid is 20min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040105A (en) * | 2015-06-06 | 2015-11-11 | 青岛科技大学 | Method for preparing calcium sulfate whiskers with oyster shells |
| CN106319631A (en) * | 2016-08-30 | 2017-01-11 | 湖北永绍科技股份有限公司 | Comprehensive treating and utilizing method of sulfuric acid waste liquor and hydrochloric acid waste liquor |
| CN106350870A (en) * | 2016-08-30 | 2017-01-25 | 湖北永绍科技股份有限公司 | Disposal and utilization method for sulfuric acid waste liquid |
| CN107663650A (en) * | 2016-07-30 | 2018-02-06 | 湖北永绍科技股份有限公司 | A kind of method that calcium sulfate crystal whiskers are prepared by shell |
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2019
- 2019-03-07 CN CN201910173097.9A patent/CN109837592B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040105A (en) * | 2015-06-06 | 2015-11-11 | 青岛科技大学 | Method for preparing calcium sulfate whiskers with oyster shells |
| CN107663650A (en) * | 2016-07-30 | 2018-02-06 | 湖北永绍科技股份有限公司 | A kind of method that calcium sulfate crystal whiskers are prepared by shell |
| CN106319631A (en) * | 2016-08-30 | 2017-01-11 | 湖北永绍科技股份有限公司 | Comprehensive treating and utilizing method of sulfuric acid waste liquor and hydrochloric acid waste liquor |
| CN106350870A (en) * | 2016-08-30 | 2017-01-25 | 湖北永绍科技股份有限公司 | Disposal and utilization method for sulfuric acid waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| "Effect of Precipitating Conditions on the Formation of Calcium-HEDP Precipitates";F. Henry Browning,et al.;《Langmuir》;19961231;第12卷;1-5 * |
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Effective date of registration: 20220110 Address after: 545000 No. 154, building 3, factory building, area a, No. 19, Chuyang Road, Liudong New District, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee after: GUANGXI YUNJI ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Address before: 545003 No. 2-248, office building, North ecological new area, Shatang Industrial Park, No. 7, Yangliu Road, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee before: Guangxi Amiba Technology Co.,Ltd. |