CN109667189A - A kind of preparation method of chrysanthemum shape precipitated calcium carbonate filler - Google Patents
A kind of preparation method of chrysanthemum shape precipitated calcium carbonate filler Download PDFInfo
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- CN109667189A CN109667189A CN201710952768.2A CN201710952768A CN109667189A CN 109667189 A CN109667189 A CN 109667189A CN 201710952768 A CN201710952768 A CN 201710952768A CN 109667189 A CN109667189 A CN 109667189A
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- calcium carbonate
- precipitated calcium
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- refining
- conductivity
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
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- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The invention discloses a kind of preparation methods of chrysanthemum shape precipitated calcium carbonate filler, include the following steps: step 1, and calcium hydroxide refining is added in carbonators, and chemical additives are added, and are uniformly mixed；Step 2 is passed through kiln gas and is carbonized, on-line checking conductivity in carbonisation, stop ventilation when conductivity reaches minimum, then increases 0.3-0.5mS/cm again, ventilates again after 5-30 minutes, until conductivity stops carbonization after being increased to 0.7-1.0mS/cm again, ripe slurry is obtained；Crystal form dressing agent is added into the ripe slurry for step 3, is uniformly mixed, the chrysanthemum shape precipitated calcium carbonate filler is obtained after cleaning.Precipitated calcium carbonate filler specific surface area with higher produced by the present invention and heavy body.It is filled with for papermaking, the indexs such as the bulk, opacity, whiteness of page can be effectively improved, while the retention of filler can be improved, fiber consumption is saved, to reduce papermaking cost.
Description
Technical field
The present invention relates to papermaking filler preparation fields, and in particular to a kind of preparation side of chrysanthemum shape precipitated calcium carbonate filler
Method.
Background technique
Precipitated calcium carbonate is one of most common filler in paper industry, substitutes paper-making fibre with filler, can reduce life
Cost is produced, optical property, printing performance and the appearance of paper in addition can be improved.Precipitated calcium carbonate is as a kind of important inorganic
Industrial chemicals may be in the different crystal morphologies such as cube, spindle, needle-shaped, chain, sheet because of the difference of preparation process.
The precipitated calcium carbonate produced with common carbonizatin method, mostly spindle-type or needle bar shape, particle size distribution range is wide, and particle is thick, dispersion
Property is bad, and covering power is bad.Chrysanthemum shape precipitated calcium carbonate is arranged by the radial growth of core of crystal seed, and such structure makes
Chrysanthemum shape precipitated calcium carbonate has very high light scattering ability, can significantly improve the whiteness and opacity of paper.Chrysanthemum shape
Precipitated calcium carbonate heavy body also with higher, the form of chrysanthemum shape can assign paper better bulk, reduce paper pulp dosage,
Reduce cost.
CN102502749A discloses a kind of method for preparing rose calcium carbonate using low-grade limestone.The invention is
Lime is prepared after long-time is calcined using the lower lime stone of calcium carbonate content, is prepared by the method for adding chemical additives
Rose-shaped winnofil.In the invention, the limestone calcination time is long, and using a variety of brightening agents, chemical additives use phosphorus
One or both of sour ammonium, citric acid rouge, also use dispersing agent, complex process, and production cost is higher.
CN105800657A discloses a kind of preparation method of rose-shaped winnofil, in burnt lime be added to
The digestion water of composite additive is digested in the ratio of 1:5-10, then crosses 60-120 mesh vibrating screen filtering and removing slag, hydrogen obtained
Chemical additives are added after being diluted with water in calcium oxide lotion, are then fed into reaction tower, are passed through after kiln gas is carbonized to pH < 7.5 and stop
Winnofil suspension is obtained rose-shaped winnofil by blocking after dehydration, drying, crushing, screening.The invention
In, it needs to add a variety of monosaccharide and polysaccharide preparation digestion water, chemical additives are also added in refining.
Though seeking the preparation process updated currently, having preparation of industrialization similar to the technique of light calcium carbonate product, simplify
Process flow reduces production cost, still has great importance.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of chrysanthemum shape precipitated calcium carbonate filler, are deposited with solving background technique
Drawbacks described above.
The present invention is achieved through the following technical solutions:
A kind of preparation method of chrysanthemum shape precipitated calcium carbonate filler, includes the following steps:
Calcium hydroxide refining is added in carbonators step 1, and chemical additives are added, and is uniformly mixed；
Step 2 is passed through kiln gas and is carbonized, on-line checking conductivity in carbonisation, when conductivity reaches minimum, so
Stop ventilation when increasing 0.3-0.5mS/cm again afterwards, ventilate again after 5-30 minutes, until conductivity is increased to 0.7-1.0mS/ again
Stop carbonization after cm, obtains ripe slurry；
Crystal form dressing agent is added into the ripe slurry for step 3, is uniformly mixed, the chrysanthemum shape lightweight is obtained after cleaning
Pearl filler.
The chemical additives are citric acid as a preferred technical solution, and additive amount is that precipitated calcium carbonate is given money as a gift quality
0.1 ‰ -3 ‰, concentration 20-30wt%.Described give money as a gift refers to water-free weight.
The crystal form dressing agent is phosphoric acid as a preferred technical solution, and additive amount is that precipitated calcium carbonate is given money as a gift quality
0.2-0.5%.
The calcium hydroxide refining is prepared with the following method as a preferred technical solution:
Calcining: step 1 obtains lime after lime stone is calcined；
Digestion: step 2 lime obtained in step (1) is digested with hot water and is slightly starched；
Removal of impurities: step 3 obtains refining through over vibration sieve and suspension separation, impurity removal after the thick slurry is thickened；
Ageing: the refining is obtained the calcium hydroxide refining by ageing by step 4.
Calcination condition in step 1 as a preferred technical solution, are as follows: use automated machine Vertical Steel kiln, lime stone
Size is 30-60mm, and coal stone ratio is 75-95kg/T lime stone, and calcination temperature controls the calcination time between 950-1050 DEG C
15-30h。
Digestion condition in step 2 as a preferred technical solution, are as follows: the mass ratio of lime and water is 1:5-1:7, is disappeared
The temperature of change is 70-90 DEG C, curing rate >=90%.
The removal of impurities in step 3, which refers to, as a preferred technical solution, is adjusted to 15-17wt% for thick slurry concentration, first passes through
100 meshes remove impurity using cyclone hydraulic separators.
Aging condition in step 4 as a preferred technical solution, are as follows: digestion time 12-24 hours, 35 DEG C -45 of temperature
℃。
In contrast to the prior art, the present invention has the advantage that and has the beneficial effect that:
1, precipitated calcium carbonate filler grain produced by the present invention is in chrysanthemum shape, specific surface area (9-15 ㎡/g) with higher
With heavy body (3-5ml/g).
2, the method for the present invention obtains chrysanthemum shape precipitated calcium carbonate filler, is filled with for papermaking, can effectively improve the pine of page
Indexs such as thickness, opacity, whiteness, while the retention of filler can be improved save fiber consumption, thus reduce papermaking at
This.
3, the method for the present invention technique is relatively easy, by on-line checking conductivity, carries out automation control reaction process, produces
Product particle diameter distribution is uniform, and quality is stablized, and realizes industrialized production.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph of chrysanthemum shape precipitated calcium carbonate filler prepared by embodiment 1.
Fig. 2 is the electromicroscopic photograph of chrysanthemum shape precipitated calcium carbonate filler prepared by embodiment 2.
Fig. 3 is the electromicroscopic photograph of chrysanthemum shape precipitated calcium carbonate filler prepared by embodiment 3.
Fig. 4 is the electromicroscopic photograph of conventional lightweight pearl filler prepared by embodiment 4.
Specific embodiment
The present invention is illustrated below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1
Using automated machine Vertical Steel kiln, selecting size is the lime stone of 30-60mm, and coal stone ratio is 80kg/T lime
Stone, calcination temperature control the calcination time 25h between 1000 DEG C.Lime is put into 80 DEG C of hot water and is digested, wherein stone
The mass ratio of ash and water is 1:6.Postdigestive thick slurry plus water adjustment concentration are 15%, 100 meshes are first passed through, using spinning liquid point
Refining is obtained after removing impurity from device.Refining cools to 45 DEG C after being aged 24 hours.Refining is squeezed into carbonators, is added 1 ‰
Citric acid (giving money as a gift relative to PCC) (concentration 30%) be used as chemical additives, stir evenly.Ventilation is carbonized, and kiln gas is dense
Degree is 30%, continuous on-line detection conductivity in carbonisation, when conductivity reaches minimum, then increases 0.5mS/cm again,
Stop ventilation.It ventilates again after five minutes, until conductivity rises 0.7mS/cm again and terminates to be carbonized.Phosphoric acid is added into ripe slurry as brilliant
Type dressing agent, additive amount are 0.3% phosphoric acid (Gu Gu /) (3Kg/ PCC per ton), are stirred evenly.It cleans by 325 meshes, finally
Obtain chrysanthemum shape light calcium carbonate slurry.Testing product solid content is 19.1%, pH 7.18, and U.S. partial size D90 is 4.102 μ
M, D50 are 1.680 μm, and specific surface area is 9.2 ㎡/g, and the body that sinks is 3.43ml/g.Product is tested and analyzed through scanning electron microscope such as Fig. 1 institute
Show.
Embodiment 2
Using automated machine Vertical Steel kiln, selecting size is the lime stone of 30-60mm, and coal stone ratio is 80kg/T lime
Stone, calcination temperature control the calcination time 25h between 1000 DEG C.Lime is put into 80 DEG C of hot water and is digested, wherein stone
The mass ratio of ash and water is 1:6.Postdigestive thick slurry plus water adjustment concentration are 15%, 100 meshes are first passed through, using spinning liquid point
Refining is obtained after removing impurity from device.Refining cools to 40 DEG C after being aged 24 hours.Refining is squeezed into carbonators, is added
1.5 ‰ citric acid (giving money as a gift relative to PCC) (concentration 30%) is used as chemical additives, stirs evenly.Ventilation is carbonized, kiln
Gas concentration is 30%, continuous on-line detection conductivity in carbonisation, when conductivity reaches minimum, then increases 0.5mS/cm again
When, stop ventilation.It ventilates again after five minutes, until conductivity rises 0.7mS/cm again and terminates to be carbonized.Phosphoric acid conduct is added into ripe slurry
Crystal form dressing agent, additive amount are 0.3% phosphoric acid (Gu Gu /) (3Kg/ PCC per ton), are stirred evenly.It cleans by 325 meshes, most
After obtain chrysanthemum shape light calcium carbonate slurry.Testing product solid content is 19.2%, pH 7.50, and U.S. partial size D90 is 3.240
μm, D50 is 1.312 μm, and specific surface area is 11.4 ㎡/g, and the body that sinks is 4.20ml/g.Product tests and analyzes such as Fig. 2 through scanning electron microscope
It is shown.
Embodiment 3
Using automated machine Vertical Steel kiln, selecting size is the lime stone of 30-60mm, and coal stone ratio is 80kg/T lime
Stone, calcination temperature control the calcination time 25h between 1000 DEG C.Lime is put into 80 DEG C of hot water and is digested, wherein stone
The mass ratio of ash and water is 1:6.Postdigestive thick slurry plus water adjustment concentration are 15%, 100 meshes are first passed through, using spinning liquid point
Refining is obtained after removing impurity from device.Refining cools to 35 DEG C after being aged 24 hours.Refining is squeezed into carbonators, is added 2 ‰
Citric acid (giving money as a gift relative to PCC) (concentration 30%) be used as chemical additives, stir evenly.Ventilation is carbonized, and kiln gas is dense
Degree is 30%, continuous on-line detection conductivity in carbonisation, when conductivity reaches minimum, then increases 0.5mS/cm again,
Stop ventilation.It ventilates again after five minutes, until conductivity rises 0.7mS/cm again and terminates to be carbonized.Phosphoric acid is added into ripe slurry as brilliant
Type dressing agent, additive amount are 0.3% phosphoric acid (Gu Gu /) (3Kg/ PCC per ton), are stirred evenly.It cleans by 325 meshes, finally
Obtain chrysanthemum shape light calcium carbonate slurry.Testing product solid content is 19.0%, pH 7.66, and U.S. partial size D90 is 2.603 μ
M, D50 are 1.108 μm, and specific surface area is 13.8 ㎡/g, and the body that sinks is 4.78ml/g.Product tests and analyzes such as Fig. 3 through scanning electron microscope
It is shown.
Embodiment 4
Using automated machine Vertical Steel kiln, selecting size is the lime stone of 30-60mm, and coal stone ratio is 80kg/T lime
Stone, calcination temperature control the calcination time 25h between 1000 DEG C.Lime is put into 80 DEG C of hot water and is digested, wherein stone
The mass ratio of ash and water is 1:6.Postdigestive thick slurry plus water adjustment concentration are 15%, 100 meshes are first passed through, using spinning liquid point
Refining is obtained after removing impurity from device.Refining cools to 35 DEG C after being aged 24 hours.Refining is squeezed into carbonators, crystal form is not added
Controlling agent stirs evenly.Ventilation is carbonized, and kiln gas concentration is 30%, and continuous on-line detection conductivity in carbonisation works as electricity
Conductance reaches minimum, when then increasing 0.5mS/cm again, stops ventilation.It ventilates again after five minutes, until conductivity rises 0.7mS/ again
Cm terminates to be carbonized, and crystal form dressing agent is not added.It cleans by 325 meshes, finally obtains conventional lightweight calcium carbonate slurry.Testing product
Solid content is 19.4%, pH 7.85, and U.S. partial size D90 is 4.496 μm, and D50 is 2.166 μm, and specific surface area is 6.0 ㎡/g,
Heavy body is 2.80ml/g.Product tests and analyzes as shown in Figure 4 through scanning electron microscope.
Paper is filled with experiment:
It selects 1 chrysanthemum light calcium sample of embodiment and the common light calcium sample of embodiment 4 to carry out paper and is filled with experiment:
Needle slurry (400SR): broad-leaved slurry (380SR)=20:80 (dry/dry) beating degree 380SR weight in wet base 3.0g
Copy paper technique: slurry (65%)+AKD (20Kg/t paper)+filler (35%)+CPAM (200ppm)
Design copy paper quantifies 80g/m2, after load weighted paper pulp is stirred 1 minute, AKD, filler, each 1 point of stirring is added
Clock, finally plus CPAM is stirred and is removed for 1 minute, with the semi-automatic sheet forming apparatus handsheet of LABTECH73-62, through LABTECH 73-50
Natural air drying after the squeezing of standard page squeezer, the indexs such as detection pattern Paper bulk, opacity, whiteness, retention.
Detection data is shown in Table 1:
Table 1
Then the present invention is by digesting limestone calcination lime, being cleaned, being aged, being regulated and controled, being carbonized and being adjusted again
The series of process processes such as control removal of impurities add phosphoric acid in ripe slurry by adding citric acid in refining as chemical additives
Automation control reaction process is carried out, chrysanthemum shape lightweight carbon is finally obtained by on-line checking conductivity as crystal form dressing agent
Sour calcium slurry.Precipitated calcium carbonate filler obtained by the present invention, shape be in chrysanthemum shape, compared with common fillers light calcium, have compared with
High specific surface area and heavy body, are filled with for papermaking, can effectively improve the indexs such as the bulk, opacity, whiteness of page, together
When the retention of filler can be improved, fiber consumption is saved, to reduce papermaking cost.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of preparation method of chrysanthemum shape precipitated calcium carbonate filler, which comprises the steps of:
Calcium hydroxide refining is added in carbonators step 1, and chemical additives are added, and is uniformly mixed；
Step 2 is passed through kiln gas and is carbonized, on-line checking conductivity in carbonisation, when conductivity reaches minimum, then again
Stop ventilation when increasing 0.3-0.5mS/cm, ventilate again after 5-30 minutes, until after conductivity is increased to 0.7-1.0mS/cm again
Stop carbonization, obtains ripe slurry；
Crystal form dressing agent is added into the ripe slurry for step 3, is uniformly mixed, the chrysanthemum shape lightweight carbonic acid is obtained after cleaning
Calcium filler.
2. the method as described in claim 1, which is characterized in that the chemical additives are citric acid.
3. method according to claim 2, which is characterized in that the additive amount of the chemical additives is given money as a gift for precipitated calcium carbonate
The 0.1 ‰ -3 ‰ of quality, concentration 20-30wt%.
4. the method as described in claim 1, which is characterized in that the crystal form dressing agent is phosphoric acid.
5. method as claimed in claim 4, which is characterized in that the additive amount of the crystal form dressing agent is given money as a gift for precipitated calcium carbonate
The 0.2-0.5% of quality.
6. the method as described in claim 1, which is characterized in that the calcium hydroxide refining is prepared with the following method:
Calcining: step 1 obtains lime after lime stone is calcined；
Digestion: step 2 lime obtained in step (1) is digested with hot water and is slightly starched；
Removal of impurities: step 3 obtains refining through over vibration sieve and suspension separation, impurity removal after the thick slurry is thickened；
Ageing: the refining is obtained the calcium hydroxide refining by ageing by step 4.
7. method as claimed in claim 6, which is characterized in that the calcination condition in step 1 are as follows: vertical using automated machine
Formula steel kiln, lime stone size be 30-60mm, coal stone ratio be 75-95kg/T lime stone, calcination temperature control 950-1050 DEG C it
Between, calcination time 15-30h.
8. method as claimed in claim 6, which is characterized in that the digestion condition in step 2 are as follows: the mass ratio of lime and water
For 1:5-1:7, the temperature of digestion is 70-90 DEG C, curing rate >=90%.
9. method as claimed in claim 6, which is characterized in that the removal of impurities in step 3, which refers to, is adjusted to 15- for thick slurry concentration
17wt% first passes through 100 meshes, removes impurity using cyclone hydraulic separators.
10. method as claimed in claim 6, which is characterized in that the aging condition in step 4 are as follows: digestion time 12-24 is small
When, 35 DEG C -45 DEG C of temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113149212A (en) * | 2021-04-22 | 2021-07-23 | 四川绵阳岷山实业集团有限公司 | Radial calcium carbonate biological filler, preparation method and application thereof in sewage treatment |
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|---|---|---|---|---|
| CN1080909A (en) * | 1993-07-15 | 1994-01-19 | 北京化工学院 | The preparation method of lamellar crystal light calcium carbonate |
| CN102432054A (en) * | 2011-09-28 | 2012-05-02 | 建德市云峰碳酸钙有限公司 | Method for producing light calcium carbonate slurry and light calcium carbonate paste |
| CN102502748A (en) * | 2011-10-20 | 2012-06-20 | 福建省万旗非金属材料有限公司 | Microwave method for preparing rose-shaped calcium carbonate |
| CN103451992A (en) * | 2013-01-10 | 2013-12-18 | 湖南皓志新材料股份有限公司 | Preparation method of super-hydrophobic self-cleaning coating for papermaking |
| CN105800657A (en) * | 2016-04-22 | 2016-07-27 | 广西合山东来化工科技有限公司 | Method for preparing rosette-like precipitated calcium carbonate |
-
2017
- 2017-10-13 CN CN201710952768.2A patent/CN109667189B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1080909A (en) * | 1993-07-15 | 1994-01-19 | 北京化工学院 | The preparation method of lamellar crystal light calcium carbonate |
| CN102432054A (en) * | 2011-09-28 | 2012-05-02 | 建德市云峰碳酸钙有限公司 | Method for producing light calcium carbonate slurry and light calcium carbonate paste |
| CN102502748A (en) * | 2011-10-20 | 2012-06-20 | 福建省万旗非金属材料有限公司 | Microwave method for preparing rose-shaped calcium carbonate |
| CN103451992A (en) * | 2013-01-10 | 2013-12-18 | 湖南皓志新材料股份有限公司 | Preparation method of super-hydrophobic self-cleaning coating for papermaking |
| CN105800657A (en) * | 2016-04-22 | 2016-07-27 | 广西合山东来化工科技有限公司 | Method for preparing rosette-like precipitated calcium carbonate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113149212A (en) * | 2021-04-22 | 2021-07-23 | 四川绵阳岷山实业集团有限公司 | Radial calcium carbonate biological filler, preparation method and application thereof in sewage treatment |
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