CN1205306A - Method of preparing polymerization aluminium chloride - Google Patents
Method of preparing polymerization aluminium chloride Download PDFInfo
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- CN1205306A CN1205306A CN 97112857 CN97112857A CN1205306A CN 1205306 A CN1205306 A CN 1205306A CN 97112857 CN97112857 CN 97112857 CN 97112857 A CN97112857 A CN 97112857A CN 1205306 A CN1205306 A CN 1205306A
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- pac
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Abstract
A process for preparing polymerized aluminium chloride (PAC), especially the method for regulating its basicity features that under the pressurization aluminium hydroxide is immersed in hydrochloric acid, the extract liquid as semi-finished product is collected, and natural calcite (20-200 meshes) is used to regulate its basicity at 0-100 deg.C to obtain finished PAC liquid used to purify water. Its advantages are high purifying effect to water.
Description
The present invention relates to the preparation method's of a kind of polymerize aluminum chloride (PAC), particularly its basicity modulator approach.
PAC is a kind of water purification agent efficiently of domestic and international widespread use, both can be used for purifying daily tap water, also can be used for handling process water or sewage etc.
As everyone knows, the method for preparing PAC has bauxite pickling process, aluminium ash pickling process, aluminium vanadine pickling process and aluminium hydroxide pickling process etc.The aluminium hydroxide method is divided into two kinds of non-pressure process and pressurizations again.Non-pressure process aluminium hydroxide is insoluble in the acid, and in order to produce the PAC of higher basicity, the reaction precipitation thing is too much, has increased the difficulty of filter operation, and product cost is also higher.The basicity that pressurization makes PAC work in-process (leach liquor) can reach about 35%, but the processing drinking water effect is undesirable, and particularly the aluminium hydroxide kind is influential to basicity.Therefore, PAC work in-process (leach liquor) generally all adopt alkaline matter to modulate its basicity, to reach product standard.Alkaline matter commonly used has: NaOH, Na
2CO
3, NH
4OH, lightweight CaCO
3(CN87103009A) etc.But, adopt the cost of above-mentioned substance modulation PAC work in-process basicity higher, the PAC that particularly modulates behind the basicity is used to purify low temperature and low turbidity water source water, and when making its drinking water standard that reaches national regulation (residual turbidity is lower than 3 degree in the water), operation easier is just bigger.For example,, add 6～8PPm medicament or exceed this scope, make in the water residual turbidity and all be higher than 3 degree and (refer to here add and use Na when the source water turbidity is 8～10 when spending
2CO
3Deng PAC behind the alkaline matter modulation basicity), yet, when removing to purify aforesaid low temperature and low turbidity water source water, just can make it reach drinking water standard (being lower than 3 degree) as long as add 6～8PPm medicament with the PAC behind the calcite modulation basicity.
The objective of the invention is to seek a kind of material that can be used to modulate PAC work in-process (leach liquor) basicity, PAC through the modulation basicity, can be used to purify the source water of high and low turbidity, its residual turbidity all is lower than below 3 degree, meet the drinking water standard that country formulates, and can obviously reduce product cost.
For finishing task of the present invention, we adopt multiple alkaline matter, go through the basicity test of the leach liquor (being liquid PAC work in-process) of modulating aluminium hydroxide and hydrochloric acid for up to a hundred times, and the liquid PAC that makes is used to purify the source water test, therefrom filter out the optimisation substance that is used to modulate PAC work in-process basicity.
It is as follows now will to prepare the PAC process prescription:
Hydrochloric acid is added in the acidproof strap clamp cover autoclave, starts agitator and add aluminium hydroxide, be warming up to 150～180 ℃ and continue to stir the settlement separate leach liquor (liquid PAC work in-process) that makes after 6～8 hours.With leach liquor and alkaline matter respectively 0 ℃～100 ℃ stirring state modulated about 2 hours, and 1～2 hour after-filtration of constant temperature slaking, the liquid PAC product that its filtrate being makes, its basicity is 60～75%.
Technical scheme of the present invention can realize like this:
Being raw material and hydrochloric acid with aluminium hydroxide depresses reaction adding, and collects its leach liquor (PAC work in-process), modulates its basicity with natural calcite under 0 ℃～100 ℃ temperature, filters the just liquid PAC finished product for making of its filtrate of back, and its basicity is 60～75%.
Technical scheme of the present invention also can realize like this:
Above-mentioned natural calcite, its granularity are 20～200 orders.
Technical scheme of the present invention can also realize like this:
(liquid PAC work in-process are with AL (OH) to be used to modulate the leach liquor of basicity
3The meter) with natural calcite (with CaCO
3Meter) ratio of weight is 1.194～1.208.
Implement technique scheme of the present invention, have the following advantages:
1, the PAC product that makes is used for purifying drinking water, no matter is low temperature and low turbidity water source water or ultra, all can reach the following drinking water standard of 3 degree of national regulation rapidly.
2, because the natural calcite low price has the obvious benefit that reduces water producing cost.
Embodiment 1. preparation PAC work in-process (the PAC work in-process of non-modulated basicity, i.e. leach liquor).
With 1800L hydrochloric acid (density 1.156g/cm
3, concentration is 31%) be added in the acidproof autoclave of strap clamp cover, under stirring state, add 1500kgAl (OH)
3(AL
2O
3Content is 64%), be warming up to 150 ℃ of reactions 6 hours, filter the liquid PAC work in-process (leach liquor) that its filtrate being makes, it must be measured and be 3m
3, its technical indicator is:
Density: 1.34g/cm
3Al
2O
3: 14%
Basicity: 43% PH～2.5
The basicity of embodiment 2. modulation PAC work in-process (leach liquor).
Embodiment 2-A:
(its density is 1.34g/cm to get PAC work in-process (leach liquor) 500ml that embodiment 1 produces
3, Al
2O
3Content is 14%, and basicity is 43%, PH～2.5) put into the 1L beaker, temperature is controlled at 0 ℃, starts to stir and the slow 140g20 of adding purpose natural calcite (CaCO
3Content is 80%), constant temperature 2.0 hours filters when bubble not had is emitted, and the 490ml filtrate that it obtains is the PAC product that makes, and its technical indicator is respectively:
Density: 1.326g/cm
3Al
2O
3Content: 12.63%
Basicity: 67.36% PH～3.5
Embodiment .2-B～2-G:
The preparation method of embodiment 2-B, 2-C, 2-D, 2-E, 2-F, 2-G liquid PAC and the consumption of process and PAC work in-process and natural calcite are all with embodiment 2-A.The technical indicator of the granularity of temperature, the natural calcite of modulation basicity and the liquid PAC product that makes is all listed in the table 1 among each embodiment.
With natural calcite, lightweight CaCO
3And Na
2CO
3Liquid PAC product (seeing Table 1～3) behind the modulation basicity is used for purifying treatment preserved egg river, and its effect is listed in respectively in table 4～9.
Be not difficult to find out that from above-mentioned table 1 when the temperature of modulation PAC basicity was high, the time of reacting used was just short, otherwise the time is just long.Also can see from table 4～9, the temperature of modulation basicity is advisable between 0 ℃～100 ℃, if it is just poor to purify the effect of source water when higher.
The effect of modulating its basicity for further checking PAC work in-process (leach liquor) lab scale, the 3m that makes according to embodiment 1
3PAC work in-process (leach liquor), the slow natural calcite (CaCO that adds 800kg under 20 ℃ of stirring states
3Content is 85%, and granularity is 30 orders), finally make 2.8m
3(its density is 1.330g/cm to liquid PAC product
3, Al
2O
3Content is 12.73%, and basicity is 70.13%, PH～3.5).The effect that PAC product behind the modulation basicity that aforementioned industrial test is made is used to purify the preserved egg river with use lightweight CaCO
3And Na
2CO
3The application result of PAC purifying treatment preserved egg river all is listed in the table 10 behind the modulation basicity.
From table 4～10 people as can be seen, the PAC that makes with the natural calcite modulation half-finished basicity of PAC is used for purifying treatment preserved egg river effect and all is better than using Na
2CO
3With lightweight CaCO
3PAC behind the modulation basicity, and, can reach the standard of tap water through sedimentation processing in 300 seconds.
The difficulty that the source water of purifying treatment low temperature and low turbidity water makes it reach drinking water standard is bigger, still, has but received the well-content effect of people (referring to table 11) in addition with the PAC behind the natural calcite modulation basicity.For example, when with the PAC purifying treatment-2 behind the natural calcite modulation basicity ℃～1 ℃ of preserved egg river, consumption only is that 6～8PPm can reach drinking water standard.But, when using Na
2CO
3Or lightweight CaCO
3When the PAC of modulation behind the basicity removed the same source water of purifying treatment, its consumption was 6～8PPm or when exceeding this scope, remaining turbidity all exceeds the standard of tap water in the water of source.
Add dose when source water turbidity fluctuation is big, can for the system water management and bring very big difficulty, yet, during with the PAC purifying treatment source water of natural calcite modulation basicity, can reach drinking water standard rapidly.
PAC work in-process with behind the natural calcite modulation basicity also can be made into solid PAC product through concentrate drying.
The table 1 that the present invention mentions～11 all are attached to the specification sheets back.
The natural calcite outward appearance is white in color, and its foreign matter content is not trigonal systems such as faint yellow, rose-colored and brown simultaneously, becomes water chestnut stone body and scalenohedron body, and vitreous luster is arranged.There is the comparison rich in natural resources in huge rock area, China Jilin Province, its price is far below other alkaline matters, when using it for the half-finished basicity of modulation PAC, its granularity generally is advisable at 20～200 orders, excessive meeting brings difficulty to operations such as sedimentation filtrations as fruit granule, and is meticulous as fruit granule, though reaction is very fast, but can bring certain difficulty to pulverizing, increase power consumption.
In a word, with natural calcite modulation PAC work in-process basicity, its technology is fairly simple feasible, and settling velocity is fast when easy handling control, purification source water, and decontamination effect improving is splendid, can obviously reduce the products production cost.Product detects through Jilin Province's quality monitoring testing station, Jilin Province health and epidemic prevention department, and its chemical index and toxicologic index are all qualified, are the efficient water-purifying agents that a kind of purifying treatment is drunk source water.
Table 1. is modulated PAC work in-process basicity result with natural calcite
| Embodiment | Refining temperature ℃ | Calcite granularity order | Modulating time h | Liquid PAC product | ??PH | ||
| Density g/cm 3 | ??A1 2O 3????％ | Basicity % | |||||
| 2-B | ??15 | ????20 | ????2.5 | ?1.326 | ?12.63 | ?67.51 | ?3.5 |
| 2-C | ??20 | ????50 | ????2.5 | ?1.320 | ?12.61 | ?67.58 | ?3.5 |
| 2-D | ??40 | ????80 | ????2.5 | ?1.320 | ?12.35 | ?68.75 | ?3.5 |
| 2-E | ??60 | ???130 | ????1.0 | ?1.316 | ?12.20 | ?69.10 | ?3.5 |
| 2-F | ??80 | ???170 | ????1.0 | ?1.315 | ?11.98 | ?69.10 | ?3.5 |
| 2-g | ??100 | ???200 | ????1.0 | ?1.310 | ?11.32 | ?71.23 | ?3.5 |
Table 2. CaCO
3Modulation PAC work in-process basicity result
| Refining temperature ℃ | Modulating time h | Liquid PAC product | |||
| Density g/cm 3 | Aluminium sesquioxide % | Basicity % | ????PH | ||
| ?????0 | ????2.5 | ????1.324 | ????11.39 | ????65.63 | ????3.5 |
| ????15 | ????2.0 | ????1.324 | ????11.39 | ????65.72 | ????3.5 |
| ????20 | ????2.0 | ????1.322 | ????11.31 | ????65.91 | ????3.5 |
| ????40 | ????2.0 | ????1.321 | ????11.27 | ????66.32 | ????3.5 |
| ????60 | ????1.5 | ????1.316 | ????11.10 | ????67.10 | ????3.5 |
| ????80 | ????1.0 | ????1.310 | ????10.89 | ????67.92 | ????3.5 |
Table 3. Na
2CO
3Modulation PAC work in-process basicity result
| Refining temperature ℃ | Modulating time h | Liquid PAC product | |||
| Density g/cm 3 | Aluminium sesquioxide % | Basicity % | ????PH | ||
| ?????0 | ????2.5 | ????1.314 | ????11.31 | ????64.32 | ????3.5 |
| ????15 | ????2.0 | ????1.314 | ????11.31 | ????64.33 | ????3.5 |
| ????20 | ????2.0 | ????1.313 | ????1?1.23 | ????64.57 | ????3.5 |
| ????40 | ????2.0 | ????1.310 | ????11.12 | ????65.10 | ????3.5 |
| ????60 | ????1.5 | ????1.304 | ????10.92 | ????66.63 | ????3.5 |
| ????80 | ????1.0 | ????1.300 | ????10.81 | ????67.32 | ????3.5 |
The table 4.0 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 420 | 10 | 1．5 | 10 | 3．5 | 10 | 3．5 |
| 5600 | 12 | 2．0 | 12 | 4．0 | 12 | 4．0 |
The table 5.15 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 420 | 10 | 1．5 | 10 | 3．5 | 10 | 3．5 |
| 5600 | 12 | 2．0 | 12 | 4．0 | 12 | 4．0 |
The table 6.20 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 420 | 10 | 1．5 | 10 | 3．5 | 10 | 3．5 |
| 5600 | 12 | 2．0 | 12 | 4．5 | 12 | 4．5 |
The table 7.40 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 420 | 10 | 1．5 | 10 | 4．0 | 10 | 4．1 |
| 5600 | 12 | 2．0 | 12 | 5．0 | 12 | 5．0 |
The table 8.60 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 420 | 10 | 2．0 | 10 | 4．5 | 10 | 4．6 |
| 5600 | 12 | 2．3 | 12 | 5．3 | 12 | 5．4 |
The table 9.80 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 420 | 10 | 3．5 | 10 | 5．8 | 10 | 5．7 |
| 5600 | 12 | 5．3 | 12 | 6．7 | 12 | 6．6 |
PAC application result synopsis behind the table 10. modulation basicity
| Source water turbidity (degree) | ????420 | ????5600 | ||||
| Modulation class | Calcite | Yellow soda ash | Light calcium carbonate | Calcite | Yellow soda ash | Light calcium carbonate |
| (PPm) put in dispensing | ????10 | ????10 | ????10 | ????12 | ????12 | ????12 |
| Settling time (second) | Residual turbidity (degree) | Residual turbidity (degree) | ||||
| ?????60 | ???10.5 | ????18.5 | ????18.2 | ????12.3 | ????19.5 | ????19.6 |
| ????120 | ????8.5 | ????15.5 | ????14.4 | ?????9.7 | ????15.6 | ????15.6 |
| ????180 | ????6.4 | ????11.5 | ????11.2 | ?????5.1 | ????11.2 | ????11.7 |
| ????300 | ????1.7 | ?????8.0 | ????7.9 | ?????1.9 | ?????7.9 | ?????8.1 |
The table 11.0 ℃ liquid PAC product application result who makes
| Source water turbidity (degree) | The natural calcite modulation | The light calcium carbonate modulation | The yellow soda ash modulation | |||
| Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | Dosage (PPm) | Residual turbidity (degree) | |
| 8．1 | 6 | 1．0 | 6 | 3．5 | 6 | 3．7 |
| 10．1 | 8 | 1．2 | 8 | 3．6 | 8 | 4．1 |
Claims (3)
1, the preparation method of a kind of polymerize aluminum chloride (PAC), mainly be that raw material and hydrochloric acid add and depresses reaction with aluminium hydroxide, collect its leach liquor (PAC finished product), it is characterized in that modulating its basicity with natural calcite at 0～100 ℃, its filtrate is the liquid PAC product for making just.
2, according to the preparation method of the described polymerize aluminum chloride of claim 1, the granularity that it is characterized in that being used to modulating the natural calcite of basicity is 20～200 orders.
3, according to the preparation method of the described polymerize aluminum chloride of claim 1, it is characterized in that being used to modulate the PAC (in aluminium sesquioxide) of basicity and the ratio of natural calcite (in lime carbonate) weight is 1: 1.194～1.208.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97112857 CN1205306A (en) | 1997-07-15 | 1997-07-15 | Method of preparing polymerization aluminium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97112857 CN1205306A (en) | 1997-07-15 | 1997-07-15 | Method of preparing polymerization aluminium chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1205306A true CN1205306A (en) | 1999-01-20 |
Family
ID=5172515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97112857 Pending CN1205306A (en) | 1997-07-15 | 1997-07-15 | Method of preparing polymerization aluminium chloride |
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| Country | Link |
|---|---|
| CN (1) | CN1205306A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317190C (en) * | 2005-04-22 | 2007-05-23 | 内蒙古大学 | High-Al13 aluminium trichloride polymer crystal and its prepn |
| CN100337923C (en) * | 2003-06-30 | 2007-09-19 | 哈尔滨工程大学 | Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate |
| CN100355656C (en) * | 2004-07-09 | 2007-12-19 | 中国石油天然气股份有限公司 | Preparation method of polyaluminum chloride with high aluminum content |
| CN100361898C (en) * | 2004-12-24 | 2008-01-16 | 中国科学院生态环境研究中心 | Method and technique for preparing Nano type sol of polyaluminium chloride in high purity |
| CN110104668A (en) * | 2019-05-30 | 2019-08-09 | 南华大学 | A kind of preparation method of polyaluminium chloride water purification agent |
| CN112174178A (en) * | 2020-10-12 | 2021-01-05 | 马鞍山健鼎化工有限公司 | Preparation process of high-purity polyaluminum chloride |
-
1997
- 1997-07-15 CN CN 97112857 patent/CN1205306A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100337923C (en) * | 2003-06-30 | 2007-09-19 | 哈尔滨工程大学 | Process for synthesizing aluminium polychhoride by evaporating residue using ethyl acetate |
| CN100355656C (en) * | 2004-07-09 | 2007-12-19 | 中国石油天然气股份有限公司 | Preparation method of polyaluminum chloride with high aluminum content |
| CN100361898C (en) * | 2004-12-24 | 2008-01-16 | 中国科学院生态环境研究中心 | Method and technique for preparing Nano type sol of polyaluminium chloride in high purity |
| CN1317190C (en) * | 2005-04-22 | 2007-05-23 | 内蒙古大学 | High-Al13 aluminium trichloride polymer crystal and its prepn |
| CN110104668A (en) * | 2019-05-30 | 2019-08-09 | 南华大学 | A kind of preparation method of polyaluminium chloride water purification agent |
| CN112174178A (en) * | 2020-10-12 | 2021-01-05 | 马鞍山健鼎化工有限公司 | Preparation process of high-purity polyaluminum chloride |
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