CN102561086B - Method for preparing spindle crystal form alkali recovery white clay - Google Patents
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- CN102561086B CN102561086B CN201210044136.3A CN201210044136A CN102561086B CN 102561086 B CN102561086 B CN 102561086B CN 201210044136 A CN201210044136 A CN 201210044136A CN 102561086 B CN102561086 B CN 102561086B
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- white clay
- alkali recovery
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/40—Production or processing of lime, e.g. limestone regeneration of lime in pulp and sugar mills
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Abstract
The invention discloses a method for preparing spindle crystal form alkali recovery white clay. Digestion reaction and caustification reaction are separately controlled; a green solution is divided into two parts for the digestion reaction and the caustification reaction respectively; the spindle crystal form alkali recovery white clay is obtained by selecting the raw material quality, optimizing the digestion and caustification reaction technology and preferably selecting and reasonably using a crystal form control agent; and the performance and the quality of the white clay are promoted, and the white clay can meet the requirements of medium and high-grade culture paper for filler performance. By the method, the problem about environmental pollution of the white clay is solved, a filler raw material is provided for the papermaking industry, the requirement of the papermaking filler market is met, and an effect of changing waste into valuable is achieved; and the method has considerable economic benefits. Moreover, the method promotes the comprehensive utilization technology of the alkali recovery white clay, and is helpful for sustainable development of the papermaking industry.
Description
Technical field
The present invention relates to a kind of method preparing spindle crystal form alkali recovery white clay, belong to alkali recovery white slime technical field of comprehensive utilization, the spindle crystal form alkali recovery white clay of preparation, the inorganic filler being suitable as medium-to-high grade Cultural Paper is used.
Background technology
White clay is by green liquor (main component Na in alkali collection causticizing reaction process
2co
3) and quick lime (main component CaO) carries out digesting and after causticizing reaction the solid sediment that generates (main component is CaCo
3), also referred to as alkali recovery white slime, be a kind of solid waste, belong to high-alkali secondary pollution.Be both at home and abroad that the large-scale enterprises in pulp and paper industry of raw material all adopts limekiln calcination method to make alkali recovery white slime regenerate quick lime with timber, recycle in causticization.But take non-wood-fiber as the enterprises in pulp and paper industry of raw material, its white clay has serious silicon obstacle to alkali collection, not easily takes calcination method reuse, and in addition, calcination method energy consumption is high, and equipment investment is large, and production cost is high, is only applicable to large-scale enterprises in pulp and paper industry.The most papermaking enterprise of China carries out landfill or stacking to alkali recovery white slime, and some selection enters rivers, causes environmental pollution, must pay huge charges for disposing pollutants simultaneously, add enterprise's production cost, and cause the waste of resource.
According to domestic and foreign literature, one of purposes of alkali recovery white slime as paper grade (stock) inorganic filler, can both solve the problem of the contaminated environment of white clay, can be again paper industry and provide filler material, meet the needs in papermaking filler market, reach the effect turned waste into wealth.The production cost of alkali recovery white slime is about 1/3 of commodity precipitated calcium carbonate, and reuse has considerable economic benefit as papermaking filler.
In prior art, the crystalline form due to alkali recovery white slime is amorphous or cube shaped, instead of the spindle crystalline structure of commodity precipitated calcium carbonate (PCC).When making cultural paper filler with it, there is retention low, the problems such as poor optical properties and physical property are not good.
As papermaking filler and quality is the developing direction of alkali recovery white slime purification techniques close to commodity spindle PCC level.In recent years, alkali recovery white slime is back to paper production line by China's number papermaking enterprise, and the alkali recovery white slime of reuse carries out the subsequent treatment such as grinding Xie Xu to be prepared.The crystalline form of China's alkali recovery white slime mostly is impalpable structure, small part also has cubical, very large with the spindle aggregation difference of commodity PCC, cause it to keep, water filtering performance and application performance poor, this seriously constrains technological progress and the application process of papermaking waste-alkali recovery white slime process.
Therefore, how preparing the alkali recovery white slime with spindle crystalline structure, is the problem of papermaking industry engineers and technicians urgently developmental research.
In the last few years, China papermaking industry engineers and technicians have done a large amount of research and developments to the process of alkali recovery white slime and utilization thereof, but mainly concentrate on the subsequent treatment of white clay, as aspects such as washing, dealkalize, grinding Xie Xuhe dehydrate, and rarely have in crystal controlling and relate to, disclosed by following patent document:
1, Chinese invention patent open (bulletin) number 101700901A, open May 05 2010 (bulletin) day " a kind of utilize the new method of paper industry white Mud Recovered from Alkali Prepare Light Calcium Carbonate " description discloses the employing of its technical scheme
fourthe mode of section causticization and overflow causticizing reaction, crystal controlling agent is added in the 3rd section and the 4th section of causticizing reaction, this crystal controlling agent changes calcium carbonate lattice paprmeter, make crystal diameter and type can arrive the requirement of artificial setting, the precipitated calcium carbonate crystal size made is even, has abandoned grinding technique.
But the weak point that the method exists is: 1., processing step is more complicated, 2., do not describe crystal control agent used, be difficult to implement; 3. the concrete crystalline form of crystal control agent used and prepared precipitated calcium carbonate is not described, because calcium carbonate crystalline form has kind more than ten, amorphous, spherical, aciculiform, bar-shaped, chain, spindle and cube etc., and crystalline form is the critical index of calcium carbonate performance, the precipitated calcium carbonate performance difference of different crystal forms is very large, and application performance is different with effect.
2, Chinese invention patent open (bulletin) number 102303885A, open January 04 2012 (bulletin) day " a kind of careless class slurrying alkali collection green liquor refines the method for white mud calcium carbonate " description discloses the method that alkali collection green liquor refines white mud calcium carbonate, adopt clear water assimilation of quicklime using, digestion reaction and causticizing reaction are separately controlled, control material ratio, reaction temperature and speed of agitator, prepared calcium carbonate is aciculiform
.
Its weak point: this important reaction factor of not mentioned reaction time in this invention; Crystal control agent is not added in preparation process; The crystalline form of prepared calcium carbonate is aciculiform.
Summary of the invention
Object of the present invention, the weak point that purport exists for above-mentioned prior art, a kind of method preparing spindle crystal form alkali recovery white clay is proposed, spindle crystal form alkali recovery white clay prepared by the method, its quality level is close to the quality level of commodity PCC, its crystalline form is regular, whiteness is high and pH stablizes, and can meet the needs of medium-to-high grade Cultural Paper filler.
For realizing the object of the invention, the technical scheme adopted is:
a kind of method preparing spindle crystal form alkali recovery white clay, comprise digestion causticization process and white clay whiting, it is characterized in that: described spindle crystal form alkali recovery white clay, its preparation method comprises the following steps: one), raw material composition, two), digestion process, three), causticization process, four), crystal controlling, five), the separation and abstersion of white clay, six), the process of residual CaO in white clay, concrete operations are as follows:
One), raw material composition and device
Raw material forms:
1., green liquor, be clarification green liquor, green liquor total alkali 80 ~ 145g/l, in NaOH, green liquor akali sulphide 3 ~ 12g/l, in NaOH, 30% ~ 100% green liquor wherein accounting for green liquor total amount is used for assimilation of quicklime using, and 0 ~ 70% green liquor of another part remainder is used for participating in causticizing reaction,
2., quick lime; CaO content>=60
%,
3., crystal control agent: phosphoric acid, natrium citricum, sucrose and one or more mix in citric acid,
4., CO
2: industrial liquid CO
2, or the flue gas after purification;
Device:
The retort of agitator, thermometer and dropping funel is housed;
Two), digestion process
In the retort that agitator, thermometer and dropping funel are housed, inject 30% ~ 100% clarification green liquor, avoid the reduction of the white liquid concentration of alkali collection using clear water assimilation of quicklime using to bring, low whipping speed 50 ~ 600rpm, reaction time 5min ~ 60min, at temperature 65 DEG C ~ 100 DEG C, obtained milk of lime, for subsequent use;
Three), causticization process
Milk of lime and remaining 0 ~ 70% clarifys a large amount of green liquor of green liquor to mix in retort and carry out causticizing reaction, mixing speed 300 ~ 1000rpm, causticization temperature 80 DEG C ~ 100 DEG C, reaction time 90min ~ 200min, obtain alkali recovery white slime suspension;
Four), crystal control agent is added
Crystal control agent is added individually or simultaneously respectively in digestion workshop section and caustic room, described crystal control agent is one or more the hybrid combining in phosphoric acid, natrium citricum, sucrose and citric acid, consumption is 0 ~ 5.0%, to the calcium carbonate quality of green liquor theory used preparation;
Five), the separation and abstersion of white clay
The product of causticization is realized being separated and carrying out the washing of white clay of white clay and white liquid by pre-coated mud filter or lime mud folter, and the white liquid reuse of gained is as the cooking liquor of slip house.White clay after washing adds water and prepares alkali recovery white slime suspension;
Six) the residual CaO preparing alkali recovery white slime, is reduced
Industrial liquid CO is passed in prepared alkali recovery white slime suspension
2, or the flue gas after purification, adjustment pH to 8.5 ~
9.5, cross 325 mesh sieves, i.e. the obtained alkali recovery white slime product with spindle crystalline structure.
Advantage and beneficial effect
Compared with prior art, method of the present invention has simple to operate, easy to implement, the advantage that cost is low.
Beneficial effect: 1, its particle shape is spindle crystalline structure, little with the spindle aggregation difference of commodity PCC, thus improve the performance of alkali recovery white slime.2, as papermaking filler, be applied in cultural paper, in page, retention is suitable with commodity PCC, and water filtering performance is good, meets the performance requirement of high protein germplasm filler.3, this technology will promote quality and the application performance of alkali recovery white slime, promote the comprehensive utilization technique of alkali recovery white slime, contribute to the sustainable development of paper industry, and achieve the object of energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is the industrial flow schematic diagram of the inventive method;
Fig. 2 and Fig. 3 is the electron microscope picture of the amorphous particle of conventional alkali recovery white slime, the spindle crystalline structure particle of commodity PCC respectively;
Fig. 4 and Fig. 5 is the electron microscope picture of the alkali recovery white slime of spindle crystalline structure prepared by the present invention.
embodiment
Below in conjunction with embodiment, the invention will be further described, but embodiments of the present invention are not limited thereto.
Embodiment 1
Refer to Fig. 1, a kind of method preparing spindle crystal form alkali recovery white clay, by 170g quick lime with in NaOH
's300g clarifies green liquor, inject lentamente and agitator is housed, mix in the retort of thermometer and dropping funel, reaction temperature 70 DEG C, reaction time is 30min, under mixing speed 300rpm condition, the digestion carrying out quick lime obtains milk of lime, then by milk of lime with clarify green liquor in the 700g of NaOH, mix at leisure, crystal control agent is not attached separately in workshop section of digestion workshop section, described crystal control agent phosphoric acid, natrium citricum, one or more hybrid combining of sucrose and citric acid, all purchased from Tianjin sky over the river Chemical Engineering Technology Co., Ltd, the present embodiment selects 1.0g phosphoric acid and 4.2g natrium citricum as crystal control agent, control causticization temperature 98 DEG C, mixing speed 400rpm, reaction time 120min, white clay realizes being separated of white clay and white liquid with clear water washing after filtration, the white liquid be separated delivers to slip house, white clay after washing obtains white clay suspension
,and pass into industrial liquid CO in backward white clay suspension
2, or the flue gas after purification
,adjustment pH to 8.5 ~ 9.5, the present embodiment design 8.5, crosses 325 mesh sieves, is spindle crystal form alkali recovery white clay product as shown in Figure 4 and Figure 5, and storage, then delivers to paper machine room and be used as papermaking filler.
Embodiment 2
A kind of method preparing spindle crystal form alkali recovery white clay, its operating procedure is same as embodiment 1, just crystal control agent is added in digestion and caustic room simultaneously, quick lime 200g, in the consumption of the clarification green liquor of NaOH for 200g and 850g, the crystal control agent that the present embodiment adds selects natrium citricum, consumption is 4.0g, reaction temperature controls at 80 DEG C, reaction time is 50min, under mixing speed 200rpm condition, the digestion carrying out quick lime obtains milk of lime, then milk of lime and 300g are clarified green liquor, in NaOH, mix at leisure, add above-mentioned crystal control agent, consumption 1.6g, control causticization temperature 98 DEG C, mixing speed 400rpm, reaction time 150min, obtained white clay suspension, and pass into industrial liquid CO in backward white clay suspension
2, or the flue gas adjustment pH to 8.5 after purification, cross 325 mesh sieves, be spindle crystal form alkali recovery white clay product as shown in Figure 4 and Figure 5, storage, then delivers to paper machine room and is used as papermaking filler.
Embodiment 3
Prepare a method for spindle crystal form alkali recovery white clay, its operating procedure is same as embodiment 2, and crystal control agent is added in digestion and caustic room simultaneously, and quick lime 200g, with NaOH
meterthe consumption 550g of clarification green liquor, the crystal control agent that the present embodiment adds selects 1.0g phosphoric acid, 2.0g natrium citricum and 1.2g citric acid, reaction temperature controls at 85 DEG C, reaction time is that under 50min, mixing speed 400rpm condition, the digestion carrying out quick lime obtains milk of lime, then milk of lime and 600g are clarified green liquor, in NaOH, mix at leisure, add 1.6g natrium citricum
,control causticization temperature 98 DEG C, mixing speed 500rpm, reaction time 90min, obtained white clay suspension, and pass into industrial liquid CO in backward white clay suspension
2, or the flue gas after purification, adjustment pH to 8.5, crosses 325 mesh sieves, is spindle crystal form alkali recovery white clay product as shown in Figure 4 and Figure 5, and storage, then delivers to paper machine room and be used as papermaking filler.
Embodiment 4
A kind of method preparing spindle crystal form alkali recovery white clay, its operating procedure is same as embodiment 1, just crystal control agent is added on separately in digestion workshop section, quick lime 170g, the consumption of clarification green liquor is 500g, in NaOH, reaction temperature controls at 85 DEG C, reaction time is 20min, under mixing speed 300rpm condition, the digestion carrying out quick lime obtains milk of lime, then by milk of lime with clarify green liquor in the 500g of NaOH and mix at leisure, the crystal control agent that the present embodiment adds selects 0.5g phosphoric acid and 0.8 natrium citricum, control causticization temperature 99 DEG C, mixing speed 400rpm, reaction time 120min, obtained white clay suspension, and pass into industrial liquid CO in backward white clay suspension
2, or the flue gas after purification, adjustment pH to 8.5, crosses 325 mesh sieves, is spindle crystal form alkali recovery white clay product as shown in Figure 4 and Figure 5, and storage, then delivers to paper machine room and be used as papermaking filler.
Embodiment 5
A kind of method preparing spindle crystal form alkali recovery white clay, its operating procedure is same as embodiment 2, just crystal control agent is added in digestion and caustic room simultaneously, quick lime 150g and in the consumption 650g of the clarification green liquor of NaOH, the crystal control agent that the present embodiment adds selects 0.5g phosphoric acid, 0.2 sucrose and 1.5g natrium citricum, reaction temperature controls at 80 DEG C, reaction time is 50min, under mixing speed 200rpm condition, the digestion carrying out quick lime obtains milk of lime, then by milk of lime with clarify green liquor in the 300g of NaOH and mix at leisure, control causticization temperature 98 DEG C, mixing speed 400rpm, reaction time 180min, obtained white clay suspension, and pass into industrial liquid CO in backward white clay suspension
2, or the flue gas after purification, adjustment pH to 8.5, crosses 325 mesh sieves, is spindle crystal form alkali recovery white clay product as shown in Figure 4 and Figure 5, and storage, then delivers to paper machine room and be used as papermaking filler.
Embodiment 6
A kind of method preparing spindle crystal form alkali recovery white clay, its operating procedure is same as embodiment 2, just crystal control agent is added in digestion and caustic room simultaneously, quick lime 200g, green liquor is clarified in the 650g of NaOH, the crystal control agent added selects 0.6g phosphoric acid and 0.9g natrium citricum, reaction temperature controls at 65 DEG C, be 40min during reaction, under mixing speed 200rpm condition, the digestion carrying out quick lime obtains milk of lime, then milk of lime is clarified green liquor with 500g to mix at leisure, add 0.4g phosphoric acid and 1.0g natrium citricum, control causticization temperature 98 DEG C, mixing speed 470rpm, reaction time 120min, obtained white clay suspension, and pass into industrial liquid CO in backward white clay suspension
2, or the flue gas after purification, adjustment pH to 8.5, crosses 325 mesh sieves, is spindle crystal form alkali recovery white clay product as shown in Figure 4 and Figure 5, and storage, then delivers to paper machine room and be used as papermaking filler.
Adopt spindle crystal form alkali recovery white clay prepared by the inventive method, its leading indicator is as shown in table 1.
Table 1
| Index name | Alkali recovery white slime |
| CaCO 3Content % | 91.3 |
| Solid content | 16.4%% |
| Crystalline form | Spindle |
| Whiteness %ISO | 91.2 |
| Average grain diameter μm | 7.08 |
| PH value | 8.6 |
| Screen over-size (325 order) % | 0.41 |
As seen from Table 1, the calcium carbonate content of the spindle crystal form alkali recovery white clay prepared by the present invention is high, whiteness is than high, particle diameter is more moderate, and pH controls stable, and 325 residue on sieves are lower, microscopic pattern is spindle crystalline form, the nothing being different from traditional alkali recovery white slime as shown in Figure 2 determines crystalline form, and similar to the spindle crystalline form of commodity precipitated calcium carbonate (PCC) as shown in Figure 3, can meet the carrier performance requirement of medium-to-high grade Cultural Paper.
The present invention is the method preparing spindle crystal form alkali recovery white clay under non-wood pulping condition, is equally applicable to the preparation of the spindle crystal form alkali recovery white clay under pulping wood condition.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (2)
1. prepare the method for spindle crystal form alkali recovery white clay for one kind, comprise digestion causticization process and white clay whiting, it is characterized in that: described spindle crystal form alkali recovery white clay, its preparation method comprises the following steps: one), raw material composition, two), digestion process, three), causticization process, four), crystal controlling, five), the separation and abstersion of white clay, six), the process of residual CaO in white clay, concrete operations are as follows:
One), raw material composition and device
Raw material forms:
1., green liquor, be clarification green liquor, green liquor total alkali 80 ~ 145g/l, in NaOH, green liquor akali sulphide 3 ~ 12g/l, in NaOH, 30% ~ 100% green liquor wherein accounting for green liquor total amount is used for assimilation of quicklime using, and being greater than 0 and being less than or equal to 70% green liquor of another part remainder is used for participating in causticizing reaction;
2., quick lime; CaO content>=60
%,
3., crystal control agent: one or more the hybrid combining in phosphoric acid, natrium citricum, sucrose and citric acid;
4., liquid CO
2: industrial liquid CO
2;
Device:
The retort of agitator, thermometer and dropping funel is housed;
Two), digestion process
In the retort that agitator, thermometer and funnel are housed, inject 30% ~ 100% clarification green liquor, avoid the reduction of the white liquid concentration of alkali collection using clear water assimilation of quicklime using to bring, low whipping speed 50 ~ 600rpm, reaction time 5min ~ 60min, at temperature 65 DEG C ~ 100 DEG C, obtained milk of lime, for subsequent use;
Three), causticization process
Milk of lime is greater than 0 with remaining and is less than or equal to 70% clarification green liquor and mix in retort and carry out causticizing reaction, mixing speed 300 ~ 1000rpm, causticization temperature 80 DEG C ~ 100 DEG C, reaction time 90min ~ 200min, obtain alkali recovery white slime suspension;
Four), crystal control agent is added
Crystal control agent is added individually or simultaneously respectively in digestion workshop section and caustic room, described crystal control agent is one or more the hybrid combining in phosphoric acid, natrium citricum, sucrose and citric acid, consumption for being greater than 0 and being less than or equal to 5.0%, to the calcium carbonate quality of green liquor used theory preparation;
Five), the separation and abstersion of white clay
The product of causticization is realized being separated and carrying out the washing of white clay of white clay and white liquid by pre-coated mud filter or lime mud folter, and the white liquid reuse of gained is as the cooking liquor of slip house, and the white clay after washing adds water and prepares alkali recovery white slime suspension;
Six) the residual CaO preparing alkali recovery white slime, is reduced
Industrial liquid CO is passed in prepared alkali recovery white slime suspension
2, adjustment pH to 8.5 ~
9.5, cross 325 mesh sieves, i.e. the obtained alkali recovery white slime product with spindle crystalline structure.
2. the method preparing spindle crystal form alkali recovery white clay according to claim 1, is characterized in that: described method is the method preparing spindle crystal form alkali recovery white clay under non-wood pulping or pulping wood condition.
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| CN102976387B (en) * | 2012-12-07 | 2014-09-03 | 陕西科技大学 | Improved preparation technology of white mud calcium carbonate for papermaking filler |
| CN103693668B (en) * | 2013-11-28 | 2015-09-16 | 广西华纳新材料科技有限公司 | A kind of Granular fine calcium carbonate and preparation method thereof |
| CN103754918A (en) * | 2013-12-25 | 2014-04-30 | 闫冉冉 | Method for preparing alkali-recovery lime mud free of components with fine particle sizes |
| CN104803405A (en) * | 2014-01-28 | 2015-07-29 | 李广 | White mud calcium carbonate treatment technology |
| CN104843758A (en) * | 2015-04-27 | 2015-08-19 | 李广 | Dealkalization and purification method used in production of precipitated calcium carbonate |
| CN108330729B (en) * | 2018-02-11 | 2021-04-20 | 山东太阳纸业股份有限公司 | White clay filler and application thereof in cultural paper machine |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1084413C (en) * | 1998-06-14 | 2002-05-08 | 艾天召 | Process for causticizing green solution of alkali recovered from black liquid of paper-making |
| JP4672531B2 (en) * | 2005-11-18 | 2011-04-20 | ダイヤニトリックス株式会社 | Green liquid processing method |
| CN101700901A (en) * | 2009-11-25 | 2010-05-05 | 王冬生 | Novel method for producing light calcium carbonate (CaCO3) from white clay generated from alkali recovering in paper-making industry |
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