CN107892720A - The preparation method of paper pulp - Google Patents
The preparation method of paper pulp Download PDFInfo
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- CN107892720A CN107892720A CN201711131181.1A CN201711131181A CN107892720A CN 107892720 A CN107892720 A CN 107892720A CN 201711131181 A CN201711131181 A CN 201711131181A CN 107892720 A CN107892720 A CN 107892720A
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- cellulose
- pulp
- paper pulp
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/06—Cellulose acetate, e.g. mono-acetate, di-acetate or tri-acetate
-
- 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
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives thereof
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention discloses a kind of preparation method of paper pulp, comprises the following steps：Step 1, cellulose is obtained, be prepared into fiber pulp, the water content of fiber pulp obtained by regulation to 50~70wt%；Step 2, excessive acetic acid acid anhydride is added into fiber pulp according to water content, reaction is hydrolyzed under conditions of temperature is not higher than 70 DEG C；Cellulose, acetic anhydride, the mass ratio of acetic acid are 1 in regulation gained hydrolyzation system：(2~3)：(8~12), esterification is carried out under conditions of temperature is more than 80 DEG C.The present invention can be directly using aqueous fibre slurry as process object; under conditions of other chemical assistants are not added; acetic anhydride process cellulose is used in aqueous phase; cellulose is modified; appropriateness introduces acetyl group; the reduction of chemical pulp crystallinity, water retention value increase, interfacial bonding strength increase, anti-long index are improved, repeatedly recycles and still works well.
Description
Technical field
The present invention relates to commercial paper technical field, is related to a kind of preparation method of paper pulp.
Background technology
Waste paper is the main raw material(s) for producing newsprint, wrapping paper and back flow liner, and waste paper pulp-making makes full use of natural money
Source, mitigate environmental pollution.However, during reuse, the processing such as waste paper experience is beaten, squeezes and dried, with reuse number
Increase, the physical strength of waste paper significantly reduces, and pulp quality declines.Research shows that the reduction of pulp quality is fine by paper pulp
The keratinization of dimension causes, i.e. chemical pulp is dried the irreversible closing of hole made in fiber finer cell wall, caused during reuse
Paper pulp swelling capacity declines, the reduction of pliability of fiber, and interfibrous combination is not close and the intensity of paper declines.Keratinization master
It is present in chemical pulp, its mechanism also has dispute, and keratinization mechanism produces Hydrogenbond mechanism, fine fibre between having microfibre
The amorphous region between lactone bond mechanism and microfibre with fiber is formed between dimension and forms cocrystallization mechanism.
At present, domestic and foreign scholars are traditionally using addition sucrose, winnofil into chemical pulp, or addition hemicellulose
Element method suppress chemical pulp in fiber keratinization so as to improve the quality of chemical pulp, increase reuse number, but effect according to
It is so undesirable.
The content of the invention
Based on this, it is necessary to for current pulp quality it is not good enough the problems such as, there is provided a kind of preparation method of paper pulp.
A kind of preparation method of paper pulp, comprises the following steps：
Step 1, fiber essence is obtained, be prepared into fiber pulp, the water content of fiber pulp obtained by regulation to 50~70wt%；
Step 2, excessive acetic acid acid anhydride is added into the fiber pulp according to the water content, in temperature not higher than 70 DEG C
Under the conditions of reaction is hydrolyzed；Cellulose, acetic anhydride, the mass ratio of acetic acid are 1 in regulation gained hydrolyzation system：(2~3)：(8
~12), esterification is carried out under conditions of temperature is more than 80 DEG C.
In wherein some embodiments, in the esterification, cellulose, acetic anhydride, the mass ratio of acetic acid are 1：(2~
3)：10.
In wherein some embodiments, the temperature of the esterification is more than 80 DEG C and no more than 95 DEG C, and the esterification is anti-
The time answered is 1~2h.
In wherein some embodiments, the temperature of the esterification is 85 DEG C, and the time of the esterification is 1h.
In wherein some embodiments, the temperature of the hydrolysis is 50~70 DEG C, and the time of the hydrolysis is 1
~2h.
In wherein some embodiments, the temperature of the hydrolysis is 60 DEG C, and the time of the hydrolysis is 1h.
A kind of paper pulp obtained above by above-mentioned preparation method.
A kind of paper product prepared using above-mentioned paper pulp.
Compared with prior art, the invention has the advantages that：
The present invention makes the cellulose in fiber pulp in hydrolyzation system by directly adding acetic anhydride into aqueous fiber pulp
In be swelled, and by cellulose, acetic anhydride, acetic acid with when temperature optimization, without cellulose be dried, nothing
It need to add under conditions of other auxiliary agents (such as concentrated sulfuric acid catalyst), hydrophobic acetyl group, second are moderately introduced on microfibre surface
Acyl group hinders the formation of microfibre cocrystallization, and water retention value, tensile index and the internal bond strength of paper pulp significantly improve, and passes through
Repeatedly still worked well after recycling.
Brief description of the drawings
Fig. 1 is the infrared light collection of illustrative plates of paper pulp esterification；
Fig. 2 is common paper pulp and the water retention value of paper pulp of the embodiment of the present invention and the relation of cycle-index；
Fig. 3 is common paper pulp and the tensile index and internal bond strength of paper pulp of the embodiment of the present invention and the pass of cycle-index
System.
Embodiment
The preparation method of paper pulp of the present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
The present embodiment provides a kind of preparation method of paper pulp, comprises the following steps：
Step 1, cellulose is obtained, be prepared into fiber pulp, the water content of fiber pulp obtained by regulation to 50~70wt%.
The content of cellulose of this step fiber pulp is 20g；The fiber pulp of this step is also pre-processed：It is i.e. first that its is dilute
It is 1.5% fibrous suspension (fibrous suspension quality is 1333g) to be interpreted into mass concentration, and 10000 are discongested in Pulp dredger
Turn, be kept completely separate fiber.
This step after the pretreatment by above-mentioned fibrous suspension be concentrated into cellulose concentration for 40wt% (i.e. concentrate after
The quality of paper pulp is 50g), wherein content of cellulose be 20g, water content be 30g (60wt%).
Step 2, acetic anhydride, regulation temperature are added into fiber pulp obtained by step 1, starts hydrolysis, esterification,
Specific implementation is as follows：
(1) fiber pulp obtained by step 1 is moved into plastic containers (this example uses polybag), adds 170ml acetic anhydrides to enter water-filling
Solution reaction, it is 60 DEG C to control hydrolysising reacting temperature, reaction time 1h, can obtain the fiber pulp containing swollen fiber；
The quality of acetic anhydride is excessive in the step (1), and such high quality ratio contributes to cellulose swollen.Acetic anhydride
Hydrolysis can be reacted in low-temperature atmosphere-pressure, it is less demanding to reaction environment, because acetic anhydride hydrolysis be exothermic reaction, to avoid height
Temperature produces boiling explosion phenomenon, adds acetic anhydride in three times, and addition is respectively 60ml, 60ml and 50ml, and the interval time of addition is
10min.By the way that acetic anhydride is added by several times in the operation, it is 60 DEG C to control temperature, and acetic anhydride can be made to keep normal hydrolysis, avoided
HTHP causes acidic hydrolysis and the acetylation of cellulose.
(2) liquid portion in the fiber pulp of step (1) containing swollen fiber is first extruded to the fiber quality concentration obtained
For 20% swollen fiber pulp (its quality is 100g, the mixture containing 80g acetic acid and acetic anhydride), then add 50ml acetic acid
Acid anhydride, now cellulose, acetic anhydride, the mass ratio of acetic acid are 1：2.5：10, temperature is esterification 1h under the conditions of 85 DEG C.
Acetyl group can moderately be introduced by step (2) esterification, control the substitution value of cellulose in 0.15~0.25
Between.
It is understood that above-mentioned steps (2) after esterification is completed, also can use distillation water washing fiber to without residual
Remaining acetic anhydride and acetic acid.
The present embodiment adds acetic anhydride in fiber pulp, makes acetic anhydride that ester occur in a mild condition with fiber surface hydroxyl
Change reaction, it is between the presence obstruction fine cellulose of acetyl group or fine on fine cellulose surface and amorphous region introducing acetyl group
The cocrystallization of amorphous region is tieed up, the keratinization phenomenon of subsequent recovery paper pulp fiber can be suppressed.
In order to embody the effect of the present embodiment, the present embodiment is also provided with the general fibre without the processing of the present embodiment method
Slurry is shown in Fig. 1 as control, the infrared light collection of illustrative plates of the two, and water conservation value changes are shown in Fig. 2, and internal bond strength, tensile index are with following
Ring uses that (recycling at this is：Paper product is made in paper pulp, the paper product is reclaimed after use and prepares chemical pulp again and is prepared with this
Paper product, so circulation) number increase present change see Fig. 3.The discovery has broken those skilled in the art to esterification
Conventional understanding, provide new departure for the modification of paper cellulose.
Embodiment 2
This example is the change case of embodiment 1, and compared with Example 1, change part is only that：Cellulose, second in step 1
Acid anhydrides, the mass ratio of acetic acid are 1：3：8.
Embodiment 3
This example is the change case of embodiment 1, and compared with Example 1, change part is only that the esterification in step 2
Temperature be 98 DEG C.
Embodiment 4
This example is the change case of embodiment 1, and compared with Example 1, change part is only that the hydrolysis in step 2
Temperature be 40 DEG C.
Inventor also connects to the performance of chemical pulp obtained by each example has gone test, and method of testing refers to conventional method, as a result such as
Shown in table 1 below：
Table 1
Comparative example 1
This example is the comparative example of embodiment 1, and compared with Example 1, contrast part is only that, cellulose, acetic anhydride, acetic acid
Mass ratio be 1：2.5：5.
As a result, the swollen degree of this example cellulose reduces, and substitution value is less than 0.15；Paper pulp tensile index is after circulating three times
13.4 (Nm/g), far below the value 21.5 (Nm/g) of embodiment 1.
Comparative example 2
This example is the comparative example of embodiment 1, and compared with Example 1, contrast part is only that, the temperature of hydrolysis is 75
℃。
As a result, the hydrolysis of this example acetic anhydride is incomplete, and substitution value is less than 0.15；The internal bond strength of paper pulp after circulating three times
For 212J/m2, far below the value 235J/m of embodiment 12。
Comparative example 3
This example is the comparative example of embodiment 1, and compared with Example 1, contrast part is only that, the temperature of esterification is 78
℃。
As a result, this example degree of being finally replaced is less than 0.15；The water retention value of paper pulp is 73% after circulating three times, far below embodiment
1 water retention value 95%.
Comparative example 4
This example is the comparative example of embodiment 1, and compared with Example 1, contrast part is only that step 2：
(1) fiber pulp pre-processed described in step 1 is dried, obtains dry fiber element；
(2) cellulose is placed directly within swelling (60 DEG C, 1h) in acetic acid.
As a result, pulp dryer causes microfibre to crystallize, and water retention value is reduced to 70% after circulating three times.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. a kind of preparation method of paper pulp, it is characterised in that comprise the following steps：
Step 1, cellulose is obtained, be prepared into fiber pulp, the water content of fiber pulp obtained by regulation to 50~70wt%；
Step 2, excessive acetic acid acid anhydride is added into the fiber pulp according to the water content, 70 DEG C of condition is not higher than in temperature
Under reaction is hydrolyzed；Cellulose, acetic anhydride, the mass ratio of acetic acid are 1 in regulation gained hydrolyzation system：(2~3)：(8~
12) esterification, is carried out under conditions of temperature is more than 80 DEG C, produces paper pulp.
2. the preparation method of paper pulp according to claim 1, it is characterised in that cellulose, acetic acid in the esterification
Acid anhydride, the mass ratio of acetic acid are 1：(2~3)：10.
3. the preparation method of paper pulp according to claim 1, it is characterised in that the temperature of the esterification is more than 80 DEG C
And no more than 95 DEG C, the time of the esterification is 1~2h.
4. the preparation method of paper pulp according to claim 3, it is characterised in that the temperature of the esterification is 85 DEG C,
The time of the esterification is 1h.
5. the preparation method of paper pulp according to claim 1, it is characterised in that the temperature of the hydrolysis is 50~70
DEG C, the time of the hydrolysis is 1~2h.
6. the preparation method of paper pulp according to claim 5, it is characterised in that the temperature of the hydrolysis is 60 DEG C,
The time of the hydrolysis is 1h.
7. the paper pulp that any one of claim 1 to 6 preparation method obtains.
8. the paper product prepared using the paper pulp described in claim 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711131181.1A CN107892720B (en) | 2017-11-15 | 2017-11-15 | Method for producing pulp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711131181.1A CN107892720B (en) | 2017-11-15 | 2017-11-15 | Method for producing pulp |
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| CN107892720A true CN107892720A (en) | 2018-04-10 |
| CN107892720B CN107892720B (en) | 2020-06-05 |
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| CN201711131181.1A Active CN107892720B (en) | 2017-11-15 | 2017-11-15 | Method for producing pulp |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108755212A (en) * | 2018-05-15 | 2018-11-06 | 昆明理工大学 | A method of repairing secondary stock or reclaimed fibre keratinization |
| CN114907492A (en) * | 2022-06-23 | 2022-08-16 | 南京林业大学 | Method for preparing bacterial cellulose precursor material and performing bacterial cellulose acylation reaction by using precursor material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108755212A (en) * | 2018-05-15 | 2018-11-06 | 昆明理工大学 | A method of repairing secondary stock or reclaimed fibre keratinization |
| CN114907492A (en) * | 2022-06-23 | 2022-08-16 | 南京林业大学 | Method for preparing bacterial cellulose precursor material and performing bacterial cellulose acylation reaction by using precursor material |
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| CN107892720B (en) | 2020-06-05 |
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