CN1299988C - Method for washing 4A zeolite crystal - Google Patents
Method for washing 4A zeolite crystal Download PDFInfo
- Publication number
- CN1299988C CN1299988C CNB2005100433140A CN200510043314A CN1299988C CN 1299988 C CN1299988 C CN 1299988C CN B2005100433140 A CNB2005100433140 A CN B2005100433140A CN 200510043314 A CN200510043314 A CN 200510043314A CN 1299988 C CN1299988 C CN 1299988C
- Authority
- CN
- China
- Prior art keywords
- washing
- stir
- wash
- stirring
- zeolite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000005406 washing Methods 0.000 title claims abstract description 131
- 239000010457 zeolite Substances 0.000 title claims abstract description 46
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 36
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 59
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 22
- 239000006210 lotion Substances 0.000 claims description 44
- 239000003513 alkali Substances 0.000 claims description 14
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract 2
- 230000003068 static effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 239000012065 filter cake Substances 0.000 description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 7
- 238000002386 leaching Methods 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 7
- 235000017550 sodium carbonate Nutrition 0.000 description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 description 7
- 239000011734 sodium Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention relates to a washing method of a 4A zeolite crystal. The crystal washing methods used in the production process of the 4A type zeolites comprises static washing and stir washing. The washing method is characterized in that carbon dioxide gases are pumped into washing liquor; particularly, the carbon dioxide gases are pumped into stir washing liquor, and the stir washing liquor is circularly used; the stir washing liquor is controlled to be with 9 to 12 g/l of Nt, and Nc-Nt=3 to 6 g/l. The washing method of the present invention is easy to operate, and the washing liquor can be circularly used so that environmental pollution caused by the discharge of the washing liquor is avoided, and the washing water consumption is greatly reduced; thus, water resources are saved, and the water saving quantity can reach 70%; the producing cost is greatly reduced, and economical benefits and social benefits are obvious.
Description
Technical field
The present invention is the washing methods of 4A zeolite crystal, is used for the crystal washing methods of 4A zeolite production process.
Background technology
The 4A zeolite is a kind of broad-spectrum product; be widely used in building, chemistry, chemical industry and the daily life; the purposes of 4A zeolite maximum is as detergent builder; can prevent that active ingredient in the washing composition from combining with calcium ions and magnesium ions in the water and lose activity; active ingredient is normally brought into play in the protection washing composition, is to prevent that bath water from polluting the important Green Product of rivers and lakes.
It mainly is synthetic with hydrothermal synthesis method under the alkali environment producing detergent use 4A zeolite both at home and abroad, and synthetic 4A zeolite must remove attachment removal alkali through hot wash.With existing technology is example, and zeolite pH value per ton drops to below 11,4～6 tons of the deionized water of needs more than 80 ℃, and these waste water are difficult to reuse, as discharging of waste liquid not only contaminate environment but also caused the waste of resource.
Summary of the invention
The object of the present invention is to provide a kind of washing methods of 4A zeolite crystal, washing lotion can be recycled, and avoids the environmental pollution of washing lotion discharging, reduces the bath water amount again greatly, and the conserve water resource reduces production costs.
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, and it is characterized in that the logical carbon dioxide that is added with in the washings.
Suitable operation is only to lead to add carbon dioxide in stirring washing lotion.
In conjunction with actual production, in order rationally to control consumption, stir washing lotion and recycle, stir in the washing lotion: full alkali concn N
TBe 9～12g/l, the difference N of carbonic acid alkali concn and full alkali concn
C-N
T=3～6g/l.But the carbon dioxide intermittent type feeds, and stirs washing lotion washing control: stir and wash liquid-solid ratio L/S=3～4.
Through the filter cake moisture of pressure filter press filtration, if moisture is higher, the temperature that circulation can be stirred washing lotion was promoted by normal temperature, is controlled at 20～50 ℃ after detection 4A zeolite stirred and washes.
The washing principle of washing methods of the present invention:
The washing of 4A zeolite is different from the washing of materials such as aluminium hydroxide, pseudo-boehmite, red mud, and these material washings are alkali cleaning wherein to be fallen or reclaim, and the washing of 4A zeolite is the pH value that will reduce product, promptly reduces OH
-Content.And OH
-With Na
+Inseparable, washing OH
-Will inevitably wash Na off
+, Na
+Be the active princlple of zeolite, allow a certain amount of attached alkali to exist simultaneously in the product 4A zeolite, the attached alkali of permission is about 0.3～0.5%.So as long as do not contain NaOH in the 4A zeolite, the pH value of product just can not surpass 11.Therefore as long as the NaOH in the attached alkali in the product is converted into Na
2CO
3There is the pH value that just can reduce product in form.
On the adhesive tape filter, adopt quiet the washing of a step normal temperature that a large amount of attached alkali cleanings is fallen, in stirring washing lotion, lead to and add carbon dioxide, be actually and use NaHCO
3In and the NaOH in the attached liquid, overcome the high problem of attached alkali of former technology, both can reduce the wash water consumption, remove wash water heating steam, the pH value of product is reduced to below 11, the assurance product is qualified.
The washing methods of 4A zeolite crystal of the present invention, simple, washing lotion can be recycled, avoid the environmental pollution of washing lotion discharging, greatly reduced the bath water amount again, saved water resources, water-saving amount can reach 70%, greatly reduces production cost, economic benefit and obvious social benefit.
Description of drawings
Fig. 1, process flow diagram of the present invention.
Embodiment
Embodiment 1
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, the logical carbon dioxide that adds in stirring washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 9g/l, N
C-N
T=3g/l (yellow soda ash 10g/l, sodium bicarbonate 4.5g/l), L/S=4, the wash temperature of stirring washing lotion is 20 ± 5 ℃.
Follow these steps to successively wash:
(1) on the adhesive tape filter, be the quiet not washing leaching cake of washing of 1 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Embodiment 2
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, the logical carbon dioxide that adds in stirring washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 11g/l, N
C-N
T=3.5g/l (yellow soda ash 12g/l, sodium bicarbonate 5g/l), L/S=3.5, the wash temperature of stirring washing lotion is 25 ± 3 ℃.
Follow these steps to successively wash:
(1) on band filter, be the quiet not washing leaching cakes of washing of 1.5 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Embodiment 3
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, the logical carbon dioxide that adds in stirring washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 10g/l, N
C-N
T=4g/l (yellow soda ash 11g/l, sodium bicarbonate 6g/l), L/S=4, the wash temperature of stirring washing lotion is 22 ± 5 ℃.
Follow these steps to successively wash:
(1) on band filter, be the quiet not washing leaching cake of washing of 1 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Embodiment 4
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, the logical carbon dioxide that adds in stirring washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 9.5g/l, N
C-N
T=5g/l (yellow soda ash 15g/l, sodium bicarbonate 5g/l), L/S=3.2, the wash temperature of stirring washing lotion is 25 ± 5 ℃.
Follow these steps to successively wash:
(1) on band filter, be the quiet not washing leaching cake of washing of 0.6 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Embodiment 5
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, the logical carbon dioxide that adds in stirring washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 11.5g/l, N
C-N
T=4.5g/l (yellow soda ash 13g/l, sodium bicarbonate 4.5g/l), L/S=3.3, the wash temperature of stirring washing lotion is 40 ± 5 ℃.
Follow these steps to successively wash:
(1) on band filter, be the quiet not washing leaching cake of washing of 1 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Embodiment 6
The washing methods of 4A crystallization of zeolites of the present invention adds carbon dioxide to quiet washing lotion with stirring to lead to respectively in the washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 10g/l, N
C-N
T=6g/l (yellow soda ash 10g/l, sodium bicarbonate 4g/l), L/S=4, the wash temperature of stirring washing lotion is 30 ± 5 ℃.
Follow these steps to successively wash:
(1) on band filter, be the quiet not washing leaching cakes of washing of 1.5 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Embodiment 7
The washing methods of 4A crystallization of zeolites of the present invention comprises and quietly washes and stir and wash, the logical carbon dioxide that adds in stirring washing lotion, and washing lotion is stirred in the preparation circulation, stirs in the washing lotion: N
TBe 12g/l, N
C-N
T=3g/l (yellow soda ash 11g/l, sodium bicarbonate 5g/l), L/S=3.8, the wash temperature of stirring washing lotion is 22 ± 3 ℃.
Follow these steps to successively wash:
(1) on band filter, be the quiet not washing leaching cake of washing of 1 times of normal temperature industry softening water of radix with 4A zeolite butt;
(2) filter cake after quiet the washing is sent into stirred washing trough and stir and wash.
The press filtration filter cake oven dry of stirring after washing promptly get the 4A zeolite product, and filtrate returning stirred washing trough, adds carbon dioxide and recycles through leading to.
Claims (5)
1, a kind of washing methods of 4A crystallization of zeolites comprises and quietly washes and stir and wash, and it is characterized in that the logical carbon dioxide that is added with in the washings.
2, the washing methods of 4A zeolite crystal according to claim 1 is characterized in that stirring the logical carbon dioxide that is added with in the washing lotion.
3, the washing methods of 4A zeolite crystal according to claim 2 is characterized in that stirring washing lotion and recycles, and stirs in the washing lotion: full alkali concn is 9～12g/l, and the carbonic acid alkali concn is 3～6g/l with the difference of full alkali concn.
4, the washing methods of 4A zeolite crystal according to claim 3 is characterized in that stirring in the washing lotion: stir and wash liquid-solid ratio L/S=3～4.
5, the washing methods of 4A zeolite crystal according to claim 4, the wash temperature that it is characterized in that stirring washing lotion is 20～50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100433140A CN1299988C (en) | 2005-04-12 | 2005-04-12 | Method for washing 4A zeolite crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100433140A CN1299988C (en) | 2005-04-12 | 2005-04-12 | Method for washing 4A zeolite crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1686802A CN1686802A (en) | 2005-10-26 |
| CN1299988C true CN1299988C (en) | 2007-02-14 |
Family
ID=35304844
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100433140A Active CN1299988C (en) | 2005-04-12 | 2005-04-12 | Method for washing 4A zeolite crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1299988C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676326A (en) * | 2012-05-16 | 2012-09-19 | 济南大学 | Method for producing phosphorus-free pulpy detergent by comprehensively utilizing 4A zeolite and production liquid waste thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530971B (en) * | 2011-12-31 | 2013-06-12 | 云南云天化国际化工股份有限公司 | Washing method of fluorine-containing silica gel |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5474753A (en) * | 1990-11-09 | 1995-12-12 | Laviosa Rhone-Poulenc | Preparation of crystalline 4A zeolites |
| CN1219505A (en) * | 1997-12-09 | 1999-06-16 | 南京大学 | Production technique for producing washing builder 4A zeolite by semi-synthesis method |
| CN1384052A (en) * | 2001-04-30 | 2002-12-11 | 上海信渊实业有限公司 | 4A-zeolite and its prepn and use |
-
2005
- 2005-04-12 CN CNB2005100433140A patent/CN1299988C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5474753A (en) * | 1990-11-09 | 1995-12-12 | Laviosa Rhone-Poulenc | Preparation of crystalline 4A zeolites |
| CN1219505A (en) * | 1997-12-09 | 1999-06-16 | 南京大学 | Production technique for producing washing builder 4A zeolite by semi-synthesis method |
| CN1384052A (en) * | 2001-04-30 | 2002-12-11 | 上海信渊实业有限公司 | 4A-zeolite and its prepn and use |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676326A (en) * | 2012-05-16 | 2012-09-19 | 济南大学 | Method for producing phosphorus-free pulpy detergent by comprehensively utilizing 4A zeolite and production liquid waste thereof |
| CN102676326B (en) * | 2012-05-16 | 2013-03-20 | 济南大学 | Method for producing phosphorus-free pulpy detergent by comprehensively utilizing 4A zeolite and production liquid waste thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1686802A (en) | 2005-10-26 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: CHINESE ALUMINIUM CO., LTD. Free format text: FORMER OWNER: SHANDONG ALUMINIUM INDUSTRY CO., LTD. Effective date: 20071019 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20071019 Address after: 100082 No. 62 North Main Street, Beijing, Xizhimen Patentee after: Aluminum Corporation of China Limited Address before: 255052 No. 1, five km road, Zhangdian District, Shandong, Zibo Patentee before: Shandong Aluminium Industry Co., Ltd. |