CN103306159B - A kind of preparation method of modification calcium silicates papermaking filler - Google Patents

A kind of preparation method of modification calcium silicates papermaking filler Download PDF

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CN103306159B
CN103306159B CN201310187827.3A CN201310187827A CN103306159B CN 103306159 B CN103306159 B CN 103306159B CN 201310187827 A CN201310187827 A CN 201310187827A CN 103306159 B CN103306159 B CN 103306159B
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calcium silicates
papermaking filler
modification
filler
preparation
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CN103306159A (en
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张美云
宋顺喜
吴养育
孙俊民
张战军
吴盼
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Shanxi Yuzhu new material Polytron Technologies Inc
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a kind of preparation method of modification calcium silicates papermaking filler, belong to pulp technology for making paper, preparation method is: get raw material calcium silicates papermaking filler, when being heated to 600 ~ 900 DEG C with the heating rate of 5 ~ 15 DEG C/min, after insulation 60 ~ 300min, obtain modification calcium silicates papermaking filler.The present invention carries out heat modification process to papermaking filler calcium silicates, strict control heating rate and temperature, through the calcium silicate filling material of modification, in conglobulation body structure, porous surface form disappears, and degree of crystallinity is good, and average grain diameter is 10 ~ 20 μm, whiteness is 85 ~ 91%ISO, and the calcination loss at 525 DEG C is 0%.The present invention is easy and simple to handle, environmental friendliness, is suitable for suitability for industrialized production.

Description

A kind of preparation method of modification calcium silicates papermaking filler
Technical field
The invention belongs to pulp technology for making paper, be specifically related to a kind of preparation method of modification calcium silicates papermaking filler.
Background technology
In order to improve paper optical property and printability, meeting some property requirement of paper, saving fibrous raw material and reducing production cost, in the production of paper, generally all needing to add filler.The amount of filling out that adds of different paper kind differs greatly, and few 2% ~ 3%, high reaches 40%.Price due to general filler only has 1/10th of string price even lower, therefore, adds more filler in paper, can significantly reduce paper production cost.Papermaking filler kind is more, and the most frequently used has powdered whiting, precipitated calcium carbonate, talcum powder, kaolin etc.The physicochemical properties of different filler are different, even if same filler, also can due to particle diameter, the difference of surface topography, its add fill out rear paper properties also can be different.
In recent years, paper producer more and more pays close attention to this index of bulk of paper.Because high bulk paper condition of equivalent thickness can substitute original heavu weights and open, not only save fibrous raw material, reduce production cost and cost of transportation simultaneously, thus bring better economic benefit for enterprise.Pertinent literature and patent report use calcium silicates effectively can improve into the bulk index of paper as papermaking filler, and it adds and fills out paper and have good optical property and strength character simultaneously.For improving into paper wadding content further, how to reduce filler just becomes technical research focus to the negative effect of paper strength.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of modification calcium silicates papermaking filler, the calcium silicate filling material through modification can improve tensile index and the burst index of paper, can be retained as the stability of paper high bulk and antiquarian preferably simultaneously.
The present invention is achieved through the following technical solutions:
The preparation method of modification calcium silicates papermaking filler of the present invention is: get raw material calcium silicates papermaking filler, when being heated to 600 ~ 900 DEG C with the heating rate of 5 ~ 15 DEG C/min, after insulation 60 ~ 300min, obtains modification calcium silicates papermaking filler.
Described when being heated to 730 ~ 850 DEG C, insulation 140 ~ 250min.
Described heat treated is carried out in high temperature furnace.
Described modification calcium silicates papermaking filler is conglobulation body structure, and porous surface form disappears, and average grain diameter is 10 ~ 20 μm, and whiteness is 85 ~ 91%, and degree of crystallinity is good, and the calcination loss at 525 DEG C is 0%.
Described raw material calcium silicates papermaking filler is hydrated calcium silicate, and in floury structure, surface is cellular form, and average grain diameter is 20 ~ 30 μm, and whiteness is 86 ~ 93%, and specific area is 80 ~ 200m 2/g, crystallization degree is bad, and the calcination loss at 525 DEG C is 8 ~ 12%.
Compared with prior art, the present invention has following useful technique effect:
The present invention carries out heat modification process to papermaking filler calcium silicates, strict control heating-up temperature and heating rate, and method is simple, low for equipment requirements, environmental friendliness, is applicable to suitability for industrialized production.
The crystal state of the raw material calcium silicates papermaking filler that the present invention uses is the filler that crystallization is bad or major part is undefined structure, after the inventive method process, the chemical composition of raw material does not change, but there is good crystal state, physical aspect there occurs larger change simultaneously, thus utilizes the calcium silicate filling material of modification to create impact to paper properties.
Adopt the calcium silicate filling material that the inventive method is modified, in conglobulation body structure, porous surface form disappears, and degree of crystallinity is good, and average grain diameter is 10 ~ 20 μm, and whiteness is 85 ~ 91%ISO, and the calcination loss at 525 DEG C is 0%.According to TAPPI standard, the physical property that handsheet detects paper is made to modified calcium silicate filling material, result shows, modified calcium silicate filling material can significantly improve the tensile strength of paper, compared with common papermaking filler, there is good bulk, simultaneously, because the moisture in modified calcium silicate filling material is removed, the DIMENSIONAL STABILITY of the paper made improves.
Accompanying drawing explanation
Fig. 1 is scanning electronic microscope (SEM) photo of the raw material calcium silicates of the embodiment of the present invention 4;
Fig. 2 is scanning electronic microscope (SEM) photo of the calcium silicate filling material of the modification of the embodiment of the present invention 4.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Raw material calcium silicates of the present invention prepares according to patent of invention " aluminous fly-ash produces the method for aluminum and coproducing active calcium silicate " (patent No. is 201110117710.9).
Embodiment 1
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 12 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface, its average grain diameter is 20 μm, and whiteness is 93%ISO, and specific area is 200m 2/ g, crystallization degree is bad, and calcination loss is 11%(525 DEG C);
2) when temperature rises to 730 DEG C, stop heating up, and after processing 160min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, porous surface form disappears, and become conglobulation body structure (as Fig. 2), its average grain diameter is 10 μm, and whiteness is 91%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Embodiment 2
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 15 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface, its average grain diameter is 23.6 μm, and whiteness is 87.6%ISO, and specific area is 160m 2/ g, crystallization degree is bad, and calcination loss is 8%(525 DEG C);
2) when temperature rises to 750 DEG C, stop heating up, and after processing 180min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, porous surface form disappears, and become conglobulation body structure, its average grain diameter is 14 μm, and whiteness is 86.7%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Embodiment 3
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 5 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface, its average grain diameter is 25 μm, and whiteness is 86%ISO, and specific area is 135m 2/ g, crystallization degree is bad, and calcination loss is 11.2%(525 DEG C).
2) when temperature rises to 780 DEG C, stop heating up, and after processing 250min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, porous surface form disappears, and become conglobulation body structure, its average grain diameter is 14.8 μm, and whiteness is 85%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Embodiment 4
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 10 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface (as Fig. 1), its average grain diameter is 27.2 μm, and whiteness is 92.2%ISO, and specific area is 121m 2/ g, crystallization degree is bad, and calcination loss is 10.7%(525 DEG C);
2) when temperature rises to 810 DEG C, stop heating up, and after processing 240min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, as shown in Figure 2, porous surface form disappears, and become conglobulation body structure, its average grain diameter is 17.3 μm, and whiteness is 91%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Embodiment 5
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 7 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface, its average grain diameter is 30 μm, and whiteness is 89.4%ISO, and specific area is 94m 2/ g, crystallization degree is bad, and calcination loss is 8.6%(525 DEG C).
2) when temperature rises to 850 DEG C, stop heating up, and after processing 140min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, porous surface form disappears, and become conglobulation body structure, its average grain diameter is 20 μm, and whiteness is 88.1%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Embodiment 6
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 10 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface, its average grain diameter is 27 μm, and whiteness is 88.1%ISO, and specific area is 90m 2/ g, crystallization degree is bad, and calcination loss is 8.8%(525 DEG C).
2) when temperature rises to 600 DEG C, stop heating up, and after processing 300min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, porous surface form disappears, and become conglobulation body structure, its average grain diameter is 22.1 μm, and whiteness is 91.4%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Embodiment 7
A preparation method for modification calcium silicates papermaking filler, comprises the following steps:
1) at room temperature, raw material calcium silicates is placed in high temperature furnace and carries out heat treated, controlling heating rate is 12 DEG C/min;
Wherein, raw material calcium silicates (calcium silicates papermaking filler) used, be hydrated calcium silicate, have cellular surface, its average grain diameter is 24 μm, and whiteness is 86.2%ISO, and specific area is 89m 2/ g, crystallization degree is bad, and calcination loss is 8.3%(525 DEG C).
2) when temperature rises to 900 DEG C, stop heating up, and after processing 60min at this temperature, obtain the calcium silicate filling material of modification.
Through the calcium silicate filling material of modification, porous surface form disappears, and become conglobulation body structure, its average grain diameter is 21.7 μm, and whiteness is 88.9%ISO, has good crystalline texture, and its calcination loss is 0%(525 DEG C).
Performance test is carried out to the modification calcium silicate filling material obtained:
Adopt cationic polyacrylamide as retention agent, make according to TAPPI standard the physical property that handsheet detects paper, under optimum modified condition, compared with unmodified filler, its result is as shown in table 1:
The handsheet paper performance test comparison result that table 1 adopts unmodified calcium silicates and modified calcium silicates papermaking filler to make
Project (unit) Modified filler Unmodified filler
Quantitatively (g/m 2 63.64 63.67
Bulk (cm 3/g) 1.63 2.00
Tensile strength (N.m/g) 40.3 35.0
Tear index (mN.m 2/g) 9.52 9.71
Bursting strength (KPa.m 2/g) 2.63 2.42
Filer content 20% 20%
Result shows, adopts modified filler can significantly improve the tensile strength of paper, and can obtain good bulk (adopt ordinary calcium carbonate to add to fill out, its bulk is 1.4 ~ 1.5cm simultaneously 3/ g).Usual packing material size is larger, the bulk of paper is also larger, but particle diameter is excessive, easily cause paper stress raisers, add the destructiveness of its paper strength, and the present invention through the filler of modification under ensureing good bulk, also there is good intensity, meanwhile, because the moisture in modified filler is removed, the dimensionally stable of the paper made by it can improve.
To sum up, the heat treatment method of modifying of a kind of calcium silicate filling material provided by the invention, that crystallization is bad or most of raw material calcium silicates for undefined structure through the inventive method process, the modification calcium silicates obtained, its chemical composition does not change, but crystal structure and physical aspect there occurs change, thus in further paper-making process, impact is created on the performance of one-tenth paper, compared with unmodified calcium silicate filling material, the modified filler of heat treatment can significantly improve the tensile index and burst index that add and fill out paper, the characteristic of paper high bulk can be retained as simultaneously preferably and maintain dimensional stability properties.
Above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or replaces on an equal basis wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.

Claims (2)

1. a preparation method for modification calcium silicates papermaking filler, is characterized in that: get raw material calcium silicates papermaking filler, when being heated to 730 ~ 850 DEG C with the heating rate of 5 ~ 15 DEG C/min, after insulation 140 ~ 250min, obtains modification calcium silicates papermaking filler; Obtained modification calcium silicates papermaking filler is conglobulation body structure, and porous surface form disappears, and average grain diameter is 10 ~ 20 μm, and whiteness is 85 ~ 91%, and degree of crystallinity is good, and the calcination loss at 525 DEG C is 0%;
Described raw material calcium silicates papermaking filler is hydrated calcium silicate, and in floury structure, surface is cellular form, and average grain diameter is 20 ~ 30 μm, and whiteness is 86 ~ 93%, and specific area is 80 ~ 200m 2/ g, crystallization degree is bad, and the calcination loss at 525 DEG C is 8 ~ 12%.
2. the preparation method of a kind of modification calcium silicates papermaking filler according to claim 1, it is characterized in that, described heat treated is carried out in high temperature furnace.
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CN105696409B (en) * 2016-04-13 2017-10-27 陕西科技大学 It is a kind of to improve the method that calcium silicates is filled with paper strength character
CN105887556B (en) * 2016-04-13 2017-10-27 陕西科技大学 It is a kind of to improve the method for being filled with paper strength character
CN106120441B (en) * 2016-06-20 2018-09-18 广州聚注通用技术研究院有限公司 A kind of modified calcium silicates papermaking filler and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1050365A (en) * 1990-10-04 1991-04-03 北京化工学院 A kind of method for preparing porous calcium silicate filler
CN1557706A (en) * 2004-01-17 2004-12-29 中国地质科学院郑州矿产综合利用研究 Method for preparing wollastonite extra white powder by using discharged waste liquid of soda production
CN101734673A (en) * 2008-11-20 2010-06-16 贵阳宝源阳光硅业有限公司 Calcium silicate and preparation method thereof
CN102173430A (en) * 2011-01-25 2011-09-07 昊青薪材(北京)技术有限公司 Technique for preparing wollastonite ultrafine powder from calcium silicate hydrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1050365A (en) * 1990-10-04 1991-04-03 北京化工学院 A kind of method for preparing porous calcium silicate filler
CN1557706A (en) * 2004-01-17 2004-12-29 中国地质科学院郑州矿产综合利用研究 Method for preparing wollastonite extra white powder by using discharged waste liquid of soda production
CN101734673A (en) * 2008-11-20 2010-06-16 贵阳宝源阳光硅业有限公司 Calcium silicate and preparation method thereof
CN102173430A (en) * 2011-01-25 2011-09-07 昊青薪材(北京)技术有限公司 Technique for preparing wollastonite ultrafine powder from calcium silicate hydrate

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