CN108191983A - A kind of method that serialization washing process produces low ash content hydroxyethyl cellulose - Google Patents
A kind of method that serialization washing process produces low ash content hydroxyethyl cellulose Download PDFInfo
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- CN108191983A CN108191983A CN201810007892.6A CN201810007892A CN108191983A CN 108191983 A CN108191983 A CN 108191983A CN 201810007892 A CN201810007892 A CN 201810007892A CN 108191983 A CN108191983 A CN 108191983A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/08—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals with hydroxylated hydrocarbon radicals; Esters, ethers, or acetals thereof
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Abstract
The invention discloses a kind of methods that serialization washing process produces low ash content hydroxyethyl cellulose, belong to field of material technology.The technical problem to be solved in the present invention is to provide a kind of production efficiency height, and cleaning solvent loss and loss of material are small, the method that low-cost serialization washing process produces low ash content hydroxyethyl cellulose.The method that serialization washing process produces low ash content hydroxyethyl cellulose, it is characterised in that:Include the following steps:A, hydroxyethyl cellulose crude product with crosslinking agent is mixed, carries out crosslinking Treatment, obtain slurry a;B, cleaning solvent is added in into slurry a obtained by step A, obtains slurry b;C, slurry c obtained by step B is added in rotary pressure centrifuge, is washed through serialization, obtain low ash content hydroxyethyl cellulose.The method of the present invention is remarkably improved working efficiency, and cleaning solvent loss and loss of material are significantly improved, and product content of ashes is substantially reduced, and is worthy of popularization.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of serialization washing process produces low ash content hydroxy ethyl fiber
The method of element.
Background technology
Hydroxyethyl cellulose is mainly used in emulsion paint production.With market apply demand, in order to improve product quality,
Increase market core competitiveness, high-end emulsion paint user proposes the quality of hydroxyethyl cellulose more strict requirements, special
It is not for ash content index, it is desirable that down to 5% and less.
In order to meet high-end customer using needs, domestic hydroxyethyl cellulose manufacturer is generally using multiple interval repeatedly
Property washing produce low ash product, used washing facility is conventional formula centrifuge, this production efficiency is relatively low, and is washed
Solvent loss and loss of material are larger.
Rotary pressure centrifuge is a kind of efficiently quick, and security performance is high, and the washing for meeting continuous production is set
It is standby, it is generally used in the low industrial circle of separation of solid and liquid difficulty.In order to which it to be smoothly used in hydroxyethyl cellulose manufacture
Industry and the low ash product of continuous production, processing that need to be Jing Guo series of process technology, the adjusting of operating mode reduce ethoxy fibre
The separating difficulty of the plain slurry of dimension, smoothly realizes the production of low ash product.
Invention content
Technical problem solved by the invention is to provide a kind of production efficiency height, and cleaning solvent loss and loss of material
Method small, that low-cost serialization washing process produces low ash content hydroxyethyl cellulose.
There is provided a kind of serialization washing process to produce for technological means used by the present invention solves above-mentioned technical problem
The method of low ash content hydroxyethyl cellulose, this method include the following steps:
A, hydroxyethyl cellulose crude product with crosslinking agent is mixed, carries out crosslinking Treatment, obtain slurry a;
B, cleaning solvent is added in into slurry a obtained by step A, obtains slurry b;
C, slurry b obtained by step B is added in rotary pressure centrifuge, is washed through serialization, obtain low ash content ethoxy
Cellulose.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step A,
The hydroxyethyl cellulose crude product is prepared by following methods:Purified cotton reacts generation alkali with sodium hydroxide in the mixed solvent
Then cellulose adds in ethylene oxide and carries out etherification reaction, adds inorganic acid and be neutralized to pH=4~8 to get ethoxy
Coarse product of cellulose.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step A,
The ash content of the hydroxyethyl cellulose crude product is 16~22%.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step A,
The crosslinking agent is glyoxal.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step A,
The dosage of the crosslinking agent is that 5~20L crosslinking agents are added in every 10000 liters of hydroxyethyl cellulose crude products.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step A,
The time of the crosslinking Treatment is 20~50min.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step B,
The cleaning solvent is useless ether-based liquid or the alcohols of C1~C3;The mass fraction of water is 10%~20% in the useless ether-based liquid.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step B,
The dosage of the cleaning solvent is regulation system solid content to 5%~10%.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step B,
After adding in cleaning solvent, 20~30min is stirred.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step C,
Strainer in the rotary pressure centrifuge uses 100~300 mesh.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step C,
The operation of serialization washing is:It is 5~10m to adjust slurry feed flow3/ h, the flow control of fresh washing lotion is in 3~8m3/
h;The alcohols that the fresh washing lotion is C1~C3 that water quality score is 10%~30%.
Wherein, serialization washing process described above is produced in the method for low ash content hydroxyethyl cellulose, in step C,
The ash content of the low ash content hydroxyethyl cellulose is 2%~5%.
Beneficial effects of the present invention:
The method of the present invention first mixes hydroxyethyl cellulose crude product with crosslinking agent, carries out crosslinking Treatment, then adds in dilution
Solvent is adjusted into the concentration of slurry before rotary pressure centrifuge, selects suitable cleaning solution, and adjustment slurry, cleaning solution are pumped into
The flow of rotary pressure centrifuge adjusts the rotating speed of rotary pressure centrifuge, to reach the low ash content hydroxyl of continuous and stable production
The purpose of ethyl cellulose;The method of the present invention is commonly washed relative to conventional centrifuge, is remarkably improved working efficiency, and washing is molten
Agent loss and loss of material are significantly improved, and product content of ashes is substantially reduced, and is worthy of popularization.
Specific embodiment
Specifically, a kind of method that serialization washing process produces low ash content hydroxyethyl cellulose, this method includes following
Step:
A, hydroxyethyl cellulose crude product with crosslinking agent is mixed, carries out crosslinking Treatment, obtain slurry A;
B, cleaning solvent is added in into slurry A obtained by step A, obtains slurry B;
C, slurry B obtained by step B is added in rotary pressure centrifuge, is washed through serialization, obtain low ash content ethoxy
Cellulose.
In the method for the present invention step A, the hydroxyethyl cellulose crude product is prepared by following methods:Purified cotton is mixing
Generation alkali cellulose is reacted with sodium hydroxide in solvent, ethylene oxide is then added in and carries out etherification reaction, add inorganic acid into
Row is neutralized to pH=4~8 to get hydroxyethyl cellulose crude product, and ash content is generally 16~22%;According to preparing hydroxyl in the art
The conventional method of ethyl cellulose crude product, wherein, mixed solvent can be C1~C3 that water quality score is 10%~18%
Alcohols;Sodium hydroxide and the mass ratio of purified cotton are 0.3~0.5:1;Ethylene oxide and the mass ratio of purified cotton are 0.8~1.2:
1;Inorganic acid is unitary, binary or ternary inorganic acid.
The method of the present invention is first using glyoxal as crosslinking agent, the general aqueous solution of glyoxal, and the mass fraction of glyoxal is
30%~50%, 5~20L crosslinking agents are added in every 10000 liters of hydroxyethyl cellulose crude products, carry out 20~50min of crosslinking Treatment,
So as to increase the extent of polymerization of hydroxyethyl cellulose molecule, increase is suspended in hydroxyethyl cellulose particle diameter in slurry system,
Be conducive to centrifuge washing to be smoothed out.
In the method for the present invention step B, the alcohols of useless ether-based liquid or C1~C3 are added in as cleaning solvent, regulation system contains admittedly
Amount is to 5%~10%, to reach successive centrifuge washing purpose;The useless ether-based liquid is to be classified washing filtering in washing facility
In, solvent that the first order filters out, the mass fraction of water is 10%~20%;The alcohols of the C1~C3 is methanol, ethyl alcohol
Deng;Using useless ether-based liquid as cleaning solvent, economize on resources, cost it is lower, it is preferred, therefore, that cleaning solvent is useless ether-based liquid;
In order to be uniformly mixed, convenient for calculating solid content, calculate solid content more accurate, after adding in cleaning solvent, optional stirring 20~
30min。
Every grade of washing is filtered for filter net type in rotary pressure centrifuge, the mode that washing lotion penetrates, and the thickness of strainer influences
The effect of washing, meticulous, filter pressure is big, cause washing resistance it is big, washing lotion is easily detected by, and washability is small, instead ash content
Also difficulty is washed, and excessively slightly, material loss is serious, causes line clogging, can also influence washing effect, therefore rotary in the method for the present invention
Pressure Centrifuges Inner filter net uses 100~300 mesh.
The present invention is adjusted into slurry before rotary pressure centrifuge by adding in retarder thinner in the actual production process
Concentration, select suitable cleaning solution, adjustment slurry, cleaning solution are pumped into the flow of rotary pressure centrifuge, and adjustment is rotary
The rotating speed of Pressure Centrifuges, the multiple countercurrent washing by equipment itself design (for logistics forward walk, and solvent slop by countercurrent washing
Inversely walk, utmostly to utilize washing lotion), to reach continuous-stable washing hydroxyethyl cellulose, it is fine to obtain low ash content ethoxy
Tie up the purpose of element.
Inventor attempts by a large amount of, determines in step C, and it is 5~10m to adjust slurry feed flow3/ h, fresh washing lotion
Flow control is in 3~8m3/h;The alcohols that the fresh washing lotion is C1~C3 that water quality score is 10%~30% passes through slurry
The adjusting of material and the flow of fresh washing lotion, controls fresh washing lotion dosage, when slurry stops conveying, you can stop adding in fresh wash
Liquid can reduce hydroxyethyl cellulose ash content to greatest extent using minimal amount of fresh washing lotion.In actual production, material is added in
Starch B, the mode of fresh washing lotion may be selected to be pumped into rotary pressure centrifuge by screw pump.
The filter that the present invention uses is a kind of rotational pressure formula filter of continuous production, the knot being fully sealed
Structure is particularly suitable for the filtering of solvent and needs the product detached in sealing is.Filter rotary drum is with certain variable speed
It is rotated in cabinet.Cyclic annular part between rotary drum and cabinet is by special coarse box closing and by separative element (separator disk)
Be separated into the region of sealing, such as filter cake collect, three times, secondary, once washing, nitrogen is dry, filter cake discharging region.Rotary drum table
There are multiple filter elements in face, and filter cake is collected into filter element and is rotated into next region with rotary drum, carries out continuous more
Secondary washing and nitrogen drying, filter cake is unloaded in region of no pressure, and is aided with filter cake discharging and filter cloth washing blowback nitrogen cleaning removing
The residue being bonded on filter cloth.
Rotary pressure centrifuge can carry out multistage continuous washing, when continuously washing series is more than or equal to 3, can obtain low
Ash content hydroxyethyl cellulose, the continuous series that washs is higher, hydroxyethyl cellulose ash content reduce it is more apparent, but cleaning solvent loss and
Loss of material is more apparent, and therefore, the continuous washing series of rotary pressure centrifuge may be selected 3~4 grades.It is continuously washed with three-level
Rotary pressure centrifuge is for example, its washing flow can divide four big steps to be operated:The first step:It is direct by product pump
The HEC slurries after thickening are inputted, carry out first order washing, discharge useless ether-based liquid;Second step:Input is from next stage washing procedure
Washing filtrate, carry out second level washing, discharge the washing filtrate of high concentration;Third walks:Fresh washing lotion is inputted, carries out the third level
Washing, discharges the washing filtrate of slight pollution, and supply upper level washing is used;4th step:It is dried, blown out using compressed gas
Cleaning solution ingredient it is condensed after be input to the use of third level washing procedure, the gas of discharge enters air-washer processing.
The present invention by a large amount of screening tests, the final ash content for preparing the low ash content hydroxyethyl cellulose of gained for 2%~
5%.
Preferably, a kind of method that serialization washing process produces low ash content hydroxyethyl cellulose, this method include following
Step:
A, it is hydroxyethyl cellulose crude product that ash content is 16~22% and glyoxal that mass fraction is 30%~50% is molten
Liquid mixes, and carries out 20~50min of crosslinking Treatment, obtains slurry a;The hydroxyethyl cellulose crude product is prepared by following methods:
Purified cotton reacts generation alkali cellulose with sodium hydroxide in the mixed solvent, then adds in ethylene oxide and carries out etherification reaction, then
It adds in inorganic acid and be neutralized to pH=4~8 to get hydroxyethyl cellulose crude product;The dosage of the glyoxal solution is every
5~20L is added in 10000 liters of hydroxyethyl cellulose crude products;
B, the useless ether-based liquid that water quality score is 10%~20% is added in into slurry a obtained by step A, regulation system contains admittedly
Amount obtains slurry b to 5%~10%;
C, slurry b obtained by step B is added in rotary pressure centrifuge, is washed through serialization, obtain ash content for 2%~
5% low ash content hydroxyethyl cellulose;The operation of serialization washing is:It is 5~10m to adjust slurry feed flow3/ h, is adopted
It is washed with fresh washing lotion, the flow control of fresh washing lotion is in 3~8m3/h;The fresh washing lotion is that water quality score is
The alcohols of 10%~30% C1~C3;The rotary pressure centrifuge Inner filter net uses 100~300 mesh.
The present invention is described in further detail below by test example and embodiment, but is not therefore protected the present invention
Scope limitation is among the embodiment described range.
Rotary pressure centrifuge employed in the embodiment of the present invention is B12 types, is bought in German BHS companies.
Embodiment 1
The method that the serialization washing process of the present embodiment produces low ash content hydroxyethyl cellulose includes the following steps:
A, 30000L hydroxyethyl celluloses crude product is mixed with the glyoxal solution that 50L mass fractions are 42% (m/m), into
Row crosslinking Treatment 20min, obtains slurry a;The hydroxyethyl cellulose crude product is prepared by following methods:Purified cotton is molten in mixing
Generation alkali cellulose is reacted in agent with sodium hydroxide, ethylene oxide is then added in and carries out etherification reaction, adds inorganic acid progress
PH=5 is neutralized to get hydroxyethyl cellulose crude product;
B, the useless ether-based liquid that water quality score is 15% is added in into slurry a obtained by step A, stirs 20min, control system
Solid content is 7%, obtains slurry b;
C, slurry b obtained by step B is pumped by screw pump in rotary pressure centrifuge, in rotary pressure centrifuge
Strainer uses 100~300 mesh, adjusts slurry feed flow 5m3/ h, fresh washing lotion are that the isopropanol that water quality score is 18% is molten
Liquid, the flow control of fresh washing lotion is in 4m3/ h, is washed through serialization, obtains low ash content hydroxyethyl cellulose, after testing, ash content
It is 4%.
Embodiment 2
The method that the serialization washing process of the present embodiment produces low ash content hydroxyethyl cellulose includes the following steps:
A, 25000L hydroxyethyl celluloses crude product with the glyoxal solution that 40L mass fractions are 40% is mixed, is handed over
Connection processing 30min, obtains slurry a;The hydroxyethyl cellulose crude product is prepared by following methods:Purified cotton is in the mixed solvent
Generation alkali cellulose is reacted with sodium hydroxide, ethylene oxide is then added in and carries out etherification reaction, add inorganic acid and neutralized
To pH=7 to get hydroxyethyl cellulose crude product;
B, the useless ether-based liquid that water quality score is 16% is added in into slurry a obtained by step A, stirs 30min, control system
Solid content is 7%, obtains slurry b;
C, slurry b obtained by step B is pumped by screw pump in rotary pressure centrifuge, in rotary pressure centrifuge
Strainer uses 100~300 mesh, and it is 7m to adjust slurry feed flow3/ h, fresh washing lotion are that the ethyl alcohol that water quality score is 22% is molten
Liquid, the flow control of fresh washing lotion is in 7m3/ h, is washed through serialization, obtains low ash content hydroxyethyl cellulose, after testing, ash content
It is 3.5%.
Embodiment 3
The method that the serialization washing process of the present embodiment produces low ash content hydroxyethyl cellulose includes the following steps:
A, 20000L hydroxyethyl celluloses crude product with the glyoxal solution that 30L mass fractions are 40% is mixed, is handed over
Connection processing 50min, obtains slurry a;The hydroxyethyl cellulose crude product is prepared by following methods:Purified cotton is in the mixed solvent
Generation alkali cellulose is reacted with sodium hydroxide, ethylene oxide is then added in and carries out etherification reaction, add inorganic acid and neutralized
To pH=6 to get hydroxyethyl cellulose crude product;
B, the useless ether-based liquid that water quality score is 18% is added in into slurry a obtained by step A, stirs 30min, control system
Solid content is 8%, obtains slurry b;
C, slurry b obtained by step B is pumped by screw pump in rotary pressure centrifuge, in rotary pressure centrifuge
Strainer uses 100~300 mesh, and it is 6m to adjust slurry feed flow3/ h, fresh washing lotion are the isopropanol that water quality score is 20%
Solution, the flow control of fresh washing lotion is in 8m3/ h, is washed through serialization, obtains low ash content hydroxyethyl cellulose, after testing, ash
It is divided into 2.5%.
Comparative example 1
The method of the present invention is shown in Table 1 with the Contrast on effect that conventional centrifuge commonly washs:
1 experimental data of table compares
By above-mentioned data it is found that carrying out continuous washing using rotary pressure centrifuge is remarkably improved working efficiency, wash
Washing solvent loss and loss of material is significantly improved, and product content of ashes is substantially reduced.
Claims (9)
1. the method that serialization washing process produces low ash content hydroxyethyl cellulose, it is characterised in that:Include the following steps:
A, hydroxyethyl cellulose crude product with crosslinking agent is mixed, carries out crosslinking Treatment, obtain slurry a;
B, cleaning solvent is added in into slurry a obtained by step A, obtains slurry b;
C, slurry b obtained by step B is added in rotary pressure centrifuge, is washed through serialization, obtain low ash content hydroxy ethyl fiber
Element.
2. the method that serialization washing process according to claim 1 produces low ash content hydroxyethyl cellulose, feature exist
In:In step A, the hydroxyethyl cellulose crude product is prepared by following methods:Purified cotton is in the mixed solvent and hydroxide
Sodium reaction generation alkali cellulose, then adds in ethylene oxide and carries out etherification reaction, add inorganic acid be neutralized to pH=4~
8 to get hydroxyethyl cellulose crude product;The ash content of the hydroxyethyl cellulose crude product is 16~22%.
3. the method that serialization washing process according to claim 1 produces low ash content hydroxyethyl cellulose, feature exist
In:In step A, the crosslinking agent is the glyoxal solution that mass fraction is 30%~50%;The dosage of the crosslinking agent is every
5~20L crosslinking agents are added in 10000 liters of hydroxyethyl cellulose crude products.
4. the method for low ash content hydroxyethyl cellulose is produced according to claims 1 to 3 any one of them serialization washing process,
It is characterized in that:In step A, the time of the crosslinking Treatment is 20~50min.
5. the method that serialization washing process according to claim 1 produces low ash content hydroxyethyl cellulose, feature exist
In:In step B, the cleaning solvent is useless ether-based liquid or the alcohols of C1~C3;The mass fraction of water is in the useless ether-based liquid
10%~20%.
6. the method for low ash content hydroxyethyl cellulose is produced according to Claims 1 to 5 any one of them serialization washing process,
It is characterized in that:In step B, the dosage of the cleaning solvent is regulation system solid content to 5%~10%.
7. the method that serialization washing process according to claim 1 produces low ash content hydroxyethyl cellulose, feature exist
In:In step C, the strainer in the rotary pressure centrifuge uses 100~300 mesh.
8. the method that serialization washing process according to claim 1 produces low ash content hydroxyethyl cellulose, feature exist
In:In step C, the operation of the serialization washing is:It is 5~10m to adjust slurry feed flow3/ h, the flow of fresh washing lotion
Control is in 3~8m3/h;The alcohols that the fresh washing lotion is C1~C3 that water quality score is 10%~30%.
9. the method for low ash content hydroxyethyl cellulose is produced according to claim 1~8 any one of them serialization washing process,
It is characterized in that:In step C, the ash content of the low ash content hydroxyethyl cellulose is 2%~5%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110156898A (en) * | 2019-05-30 | 2019-08-23 | 山东一滕新材料股份有限公司 | A method of preparing hydroxyethyl cellulose |
CN112812898A (en) * | 2020-12-31 | 2021-05-18 | 山东天和纸业有限公司 | Organic solvent method cellulose detergent and cellulose preparation method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102492044A (en) * | 2011-12-05 | 2012-06-13 | 泸州北方化学工业有限公司 | Method for refining hydroxyethylcellulose |
CN204138574U (en) * | 2014-09-11 | 2015-02-04 | 杭州弘博新材料有限公司 | The washing device applied in a kind of Xylo-Mucine production process |
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2018
- 2018-01-04 CN CN201810007892.6A patent/CN108191983A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102492044A (en) * | 2011-12-05 | 2012-06-13 | 泸州北方化学工业有限公司 | Method for refining hydroxyethylcellulose |
CN204138574U (en) * | 2014-09-11 | 2015-02-04 | 杭州弘博新材料有限公司 | The washing device applied in a kind of Xylo-Mucine production process |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110156898A (en) * | 2019-05-30 | 2019-08-23 | 山东一滕新材料股份有限公司 | A method of preparing hydroxyethyl cellulose |
CN110156898B (en) * | 2019-05-30 | 2020-08-07 | 山东一滕新材料股份有限公司 | Method for preparing hydroxyethyl cellulose |
CN112812898A (en) * | 2020-12-31 | 2021-05-18 | 山东天和纸业有限公司 | Organic solvent method cellulose detergent and cellulose preparation method |
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