CN110104668A - A kind of preparation method of polyaluminium chloride water purification agent - Google Patents

A kind of preparation method of polyaluminium chloride water purification agent Download PDF

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Publication number
CN110104668A
CN110104668A CN201910461838.3A CN201910461838A CN110104668A CN 110104668 A CN110104668 A CN 110104668A CN 201910461838 A CN201910461838 A CN 201910461838A CN 110104668 A CN110104668 A CN 110104668A
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CN
China
Prior art keywords
water purification
purification agent
polyaluminium chloride
chloride water
diaspore
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Pending
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CN201910461838.3A
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Chinese (zh)
Inventor
刘三军
刘永
王清良
李向阳
史文革
罗明亮
雷治武
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University of South China
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University of South China
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Priority to CN201910461838.3A priority Critical patent/CN110104668A/en
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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
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/56Chlorides
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a kind of preparation methods of polyaluminium chloride water purification agent, including diaspore is ground into particle;Roasting destroys the crystal structure of diaspore particle;It is sieved and carries out acidleach;The step of being refiltered after filtering and adjusting pH value;Belong to water purification agent and prepare correlative technology field, which is that polyaluminum chloride aqueous solution is made after ground, roasting, acidleach, filtering using diaspore as raw material, and preparation process is simple, high conversion rate, raw material availability are high, can save production cost.

Description

A kind of preparation method of polyaluminium chloride water purification agent
[technical field]
The invention belongs to water purification agent correlative technology fields, and in particular to a kind of preparation method of polyaluminium chloride water purification agent.
[background technique]
Aluminium polychloride (PAC) is also referred to as aluminium chloride, is the basic salt of alchlor, is a kind of inorganic polymer flocculation Agent, because it is excellent with flocculating property, sinking speed is fast, it is adaptable, throwing amount is few, and water purification is at low cost the features such as be widely used in The processing of the industrial wastewaters such as drinking water, city and chemical industry, metallurgy, petroleum.As China's strategy of sustainable development policy and water provide The implementation of source Law on Environmental Protection, to the market demand of water purification agent aluminium polychloride also will cumulative year after year whole nation dosage annual Ten thousand tons of 100-150 or so.
Ore concentration of bauxite ore handling capacity is big, and tailing yield is high, and yield was already close to 50%, 2017 year, ore concentration of bauxite Factory and office manage about 30,000,000 tons of raw ore, 1200 tons of milltailings or so are generated, in addition the bauxite gangue in nearly more than 10 year, total tailing amount At 100,000,000 tons or more, as ore concentration of bauxite treating capacity increases, tailing heap storage is increasing always.Bauxite gangue fine size, contains Water is high, and the solution of the processing of milltailings never, directly stockpiling, unloading occupy tract, so that script high expensive Ore concentration of bauxite make the matter worse.
In ore concentration of bauxite, diaspore is one of main component, and diaspore is rich in aluminium oxide, and on a small quantity Iron, manganese element develop the method that diaspore is directly prepared into polyaluminium chloride water purification agent, on the one hand can give polyaluminium Aluminium water purifying agent provides new raw material sources, on the one hand can consume a large amount of bauxite gangues, reduces because of bauxite gangue zone of illuviation The environmental problem come.
[summary of the invention]
In order to solve above-mentioned technical problem in the prior art, the present invention provides a kind of systems of polyaluminium chloride water purification agent Preparation Method, this method use diaspore as raw material, polyaluminium chloride water purification agent are made after processing, and preparation process is simple And feed stock conversion is high, technical scheme is as follows:
A kind of preparation method of polyaluminium chloride water purification agent, includes the following steps:
S1: diaspore is ground into the particle that partial size is 5-100 μm;
S2: the roasting temperature by the particle at 500-800 DEG C destroys its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium Enough hydrochloric acid is added in stone powder to be reacted;
S4: after S3 fully reacting, filtering precipitate is added calcium carbonate in filtrate and adjusts filtrate pH value, refilters, the Filtrate obtained by secondary filter is polyaluminium chloride water purification agent.
Further, in the S2, calcining time 30-150min.
Further, concentration of hydrochloric acid described in the S3 is 20%.
Further, the temperature of acidleach is 50-100 DEG C in the S3.
Further, the time of acidleach is 0.5-3h in the S3.
Further, the diaspore derives from bauxite gangue.
Compared to the prior art, the beneficial effects of the present invention are:
The present invention uses diaspore as raw material, roasts raw material in advance to destroy its crystal structure, aluminium oxide and salt Acid is reacted, and reaction can be divided into three dissolution, hydrolysis, polymerization processes.With the dissolution of aluminium and hydrochloric acid in diaspore Consumption promote water of coordination to hydrolyze so that the pH value in solution gradually rises, the hydrochloric acid for hydrolyzing generation promotes aluminium again Dissolution reaction;Meanwhile in continuous hydrolytic process, polymerization of building bridge can occur between two adjacent aluminium hydrolyzation morphologies again, so that hydrolysis The concentration of product reduces, and as a result promotes the progress of hydrolysis again;In entire reaction process, dissolution, hydrolysis, polymerization mutually intersection It replaces, develops reaction towards aluminum concentration, high basicity direction, the following are the reactions that aluminium dissolution, hydrolysis, polymerization process occur:
Dissolution: Al2O3+6H+→2Al++3H2O;
Hydrolysis: AlCl3+H2O→Al(OH)mCln+H+;
Polymerization: Al (OH) mCln → [Al2(OH)nCl6-n·XH2O)]m;
Wherein, 1≤n≤5, m≤10.
The molecular formula of diaspore of the present invention is Al2O3·H2O, containing a small amount of iron, manganese etc., using diaspore as original Material prepares polyaluminium chloride water purification agent, and raw material can effectively reduce raw material substantially with fully reacting, high conversion rate and utilization rate height Use.
[Detailed description of the invention]
Fig. 1 is preparation flow figure of the invention.
[specific embodiment]
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not For limiting the present invention.
Embodiment 1
As shown in Figure 1, a kind of preparation method of polyaluminium chloride water purification agent, comprising the following steps:
S1: diaspore is ground into the particle that partial size is 50-100 μm;
S2: the roasting temperature 1h by the particle at 500 DEG C, to destroy its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium The hydrochloric acid that enough concentration is 20% is added in stone powder, reaction 1.5h is carried out at 70 DEG C;
S4: after S3 fully reacting, filtering precipitate, it is 5 that calcium carbonate is added in filtrate and adjusts filtrate pH value, after Filter, second of filtering gained filtrate is polyaluminium chloride water purification agent.
Obtained aluminium polychloride (PAC) is subjected to correlated performance test:
One, aluminium polychloride obtained is measured using the method in " GB/T22627-2008 water treatment agent polyaluminium chloride " The indexs such as alumina content and basicity, the Testing index of the product are as shown in table 1, it is seen then that polymerization chlorine prepared by the present invention Change aluminium to be up to state standards GB/T22627-2014.
The Testing index of 1 aluminium polychloride of table
Two, the water purification performance of polymeric aluminum chlorides solution is tested
7 parts of 250mL steel plant sewage are taken, water sample pH value is adjusted with hydrochloric acid and/or sodium hydroxide, is added different amounts of PAC, quiescent settling after stirring take appropriate supernatant at subsurface 2-3cm, measure its absorbance respectively, the results are shown in Table 2 institutes Show.
2 difference PAC dosage of table handles trade effluent experimental result
Number 1 2 3 4 5 6
PAC dosage/mL 0 0.2 0.5 1 1.5 2
Absorbance A680 0.098 0.024 0.015 0.056 0.090 0.085
Turbidity/NTU 78.12 14.25 7.45 48.78 73.26 69.82
As shown in table 2, illustrate that PAC prepared by the present invention has certain water purification ability;When sewage PAC dosage is When 0.5mL/L, water purification ability is best.
Embodiment 2
A kind of polyaluminium chloride water purification agent, preparation method are as follows:
S1: diaspore is ground into the particle that partial size is 30-50 μm;
S2: the roasting temperature 1.5h by the particle at 800 DEG C, to destroy its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium The hydrochloric acid that enough concentration is 20% is added in stone powder, reaction 1.5h is carried out at 50 DEG C;
S4: after S3 fully reacting, filtering precipitate, it is 5 that calcium carbonate is added in filtrate and adjusts filtrate pH value, after Filter, second of filtering gained filtrate is polyaluminium chloride water purification agent.
Embodiment 3
A kind of polyaluminium chloride water purification agent, preparation method are as follows:
S1: diaspore is ground into the particle that partial size is 5-20 μm;
S2: the roasting temperature 2.5h by the particle at 600 DEG C, to destroy its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium The hydrochloric acid that enough concentration is 20% is added in stone powder, reaction 0.5h is carried out at 100 DEG C;
S4: after S3 fully reacting, filtering precipitate, it is 5 that calcium carbonate is added in filtrate and adjusts filtrate pH value, after Filter, second of filtering gained filtrate is polyaluminium chloride water purification agent.
Embodiment 4
A kind of polyaluminium chloride water purification agent, preparation method are as follows:
S1: diaspore is ground into the particle that partial size is 50-100 μm;
S2: the roasting temperature 1.5h by the particle at 700 DEG C, to destroy its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium The hydrochloric acid that enough concentration is 20% is added in stone powder, reaction 2h is carried out at 85 DEG C;
S4: after S3 fully reacting, filtering precipitate, it is 5 that calcium carbonate is added in filtrate and adjusts filtrate pH value, after Filter, second of filtering gained filtrate is polyaluminium chloride water purification agent.
Embodiment 5
A kind of polyaluminium chloride water purification agent, preparation method are as follows:
S1: diaspore is ground into the particle that partial size is 30-50 μm;
S2: the roasting temperature 1h by the particle at 650 DEG C, to destroy its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium The hydrochloric acid that enough concentration is 20% is added in stone powder, reaction 1.5h is carried out at 80 DEG C;
S4: after S3 fully reacting, filtering precipitate, it is 5 that calcium carbonate is added in filtrate and adjusts filtrate pH value, after Filter, second of filtering gained filtrate is polyaluminium chloride water purification agent.
Embodiment 6
A kind of polyaluminium chloride water purification agent, preparation method are as follows:
S1: diaspore is ground into the particle that partial size is 5-20 μm;
S2: the roasting temperature 1h by the particle at 500 DEG C, to destroy its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the hydraulic aluminium The hydrochloric acid that enough concentration is 20% is added in stone powder, reaction 1.5h is carried out at 70 DEG C;
S4: after S3 fully reacting, filtering precipitate, it is 5 that calcium carbonate is added in filtrate and adjusts filtrate pH value, after Filter, second of filtering gained filtrate is polyaluminium chloride water purification agent.
The above content is combine specific optimal technical scheme further detailed description of the invention, and it cannot be said that Specific implementation of the invention is only limited to these instructions.For the professional technician of the technical field of the invention, Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention Protection scope.

Claims (6)

1. a kind of preparation method of polyaluminium chloride water purification agent, which comprises the steps of:
S1: diaspore is ground into the particle that partial size is 5-100 μm;
S2: the roasting temperature by the particle at 500-800 DEG C destroys its granule crystal structure;
S3: the particle after being fired in S2 sieves with 100 mesh sieve, and obtains diaspore powder, in the diaspore powder Enough hydrochloric acid is added in end to be reacted;
S4: after S3 fully reacting, filtering precipitate is added calcium carbonate in filtrate and adjusts filtrate pH value, refilters, and second Filtering gained filtrate is polyaluminium chloride water purification agent.
2. the preparation method of polyaluminium chloride water purification agent according to claim 1, which is characterized in that in the S2, roasting Time is 30-150min.
3. the preparation method of polyaluminium chloride water purification agent according to claim 1, which is characterized in that salt described in the S3 Acid concentration is 20%.
4. the preparation method of polyaluminium chloride water purification agent according to claim 1, which is characterized in that acidleach in the S3 Temperature is 50-100 DEG C.
5. the preparation method of polyaluminium chloride water purification agent according to claim 1, which is characterized in that acidleach in the S3 Time is 0.5-3h.
6. the preparation method of polyaluminium chloride water purification agent according to claim 1, which is characterized in that the diaspore From bauxite gangue.
CN201910461838.3A 2019-05-30 2019-05-30 A kind of preparation method of polyaluminium chloride water purification agent Pending CN110104668A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5156564A (en) * 1974-11-11 1976-05-18 Oji Paper Co
CN1205306A (en) * 1997-07-15 1999-01-20 吉林化学工业公司龙江净水剂厂 Method of preparing polymerization aluminium chloride
CN101475268A (en) * 2009-02-02 2009-07-08 沈培忠 Water purification agent used under normal temperature
CN105600895A (en) * 2015-12-30 2016-05-25 西安科技大学 Method using gangue to process slime water
CN107915245A (en) * 2017-12-12 2018-04-17 青岛市昌斯达环保科技有限公司 A kind of production method and technique of high-performance polyaluminium chloride

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5156564A (en) * 1974-11-11 1976-05-18 Oji Paper Co
CN1205306A (en) * 1997-07-15 1999-01-20 吉林化学工业公司龙江净水剂厂 Method of preparing polymerization aluminium chloride
CN101475268A (en) * 2009-02-02 2009-07-08 沈培忠 Water purification agent used under normal temperature
CN105600895A (en) * 2015-12-30 2016-05-25 西安科技大学 Method using gangue to process slime water
CN107915245A (en) * 2017-12-12 2018-04-17 青岛市昌斯达环保科技有限公司 A kind of production method and technique of high-performance polyaluminium chloride

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
朱洪法: "《精细化工产品配方与制造 第4册》", 31 July 1998, 北京:金盾出版社 *
杨华明等: "《硅酸盐矿物精细化加工基础与技术》", 30 April 2012 *

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Application publication date: 20190809