CN106480780A - A kind of paper making intensifier based on hemicellulose and preparation method and application - Google Patents
A kind of paper making intensifier based on hemicellulose and preparation method and application Download PDFInfo
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- CN106480780A CN106480780A CN201610939162.0A CN201610939162A CN106480780A CN 106480780 A CN106480780 A CN 106480780A CN 201610939162 A CN201610939162 A CN 201610939162A CN 106480780 A CN106480780 A CN 106480780A
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- xylan
- hemicellulose
- paper making
- acrylamide
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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
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/18—Reinforcing agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a kind of paper making intensifier based on hemicellulose and preparation method and application.The method is comprised the following steps：Xylan is dissolved in ultra-pure water, heating for dissolving in water-bath, leads to nitrogen, initiator is added, after causing certain time, grafted monomers acrylamide is added, the cooling of rear product has been reacted, has been washed with acetone, then vacuum drying obtains crude product.Dry crude product is put into acetic acid with immersion in ethylene glycol mixture repeatedly, then vacuum drying obtains the high xylan grafted polyacrylamide of purity.The xylan grafted polyacrylamide has xylan and polyacrylamide performance concurrently, and price is less expensive, flocculability is good, effectively improves the paper performance of secondary stock.It is easy to operate that the preparation method of the present invention has technique, eco-friendly characteristic.
Description
Technical field
The present invention relates to paper making intensifier field, and in particular to a kind of paper making intensifier based on hemicellulose and its preparation
Method and application.
Background technology
Continuous deterioration due to the progressively exhausted and environmental problem of fossil resource.Agricultural-forestry biomass have environmental friendliness, can
The advantages of biodegradable, regeneration period is short.Prepared using agricultural wastes and be considered to solve environment with high valuable chemicals
One of and the effective way of energy problem.
Xylan grafted polyacrylamide, is xylan derivative after being chemically modified, by xylan and acrylamide
High temperature graft copolymerization is obtained, and possesses the strong flocculability of polyacrylamide, has very strong flocculating effect to the solute in solution, and poly-
There is amide groups in acrylamide, can form hydrogen bond with cellulose, to the effective raising of size performance, therefore can apply to make
Paper industry.Xylan grafted polyacrylamide prepared by the method has environment friendly, and environmental pollution is little.
In recent years, the deep processing of living beings receives the concern of many scientific workers, the wherein graft copolymerization of living beings
Method of modifying is particularly noticeable.Living beings graft copolymerization includes, the graft copolymerization of cellulose, the graft copolymerization of hemicellulose,
Graft copolymerization of shitosan etc..Living beings after grafting, copolymerization and modification have the superperformance of grafted monomers, make living beings
Range of application is more extensive, becomes the focus of domestic and international research.Traditional papermaking is replaced to strengthen using xylan graft acrylamide
Agent greatly reduces the shortcomings of production cost, environmental pollution, feasibility with technology and economically.
Content of the invention
In place of solving the shortcoming and defect of above prior art, it is an object of the invention to provide a kind of fine based on half
Paper making intensifier of dimension element and preparation method and application.The xylan grafted polyacrylamide has xylan and polyacrylamide concurrently
Amine performance, price is less expensive, flocculability is good, effectively improves the paper performance of secondary stock.The preparation method of the present invention has technique
Easy to operate, environment friendly.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of the paper making intensifier based on hemicellulose, comprises the steps：
(1) xylan graft copolymerization：Weigh xylan powder to be dissolved in ultra-pure water, heating for dissolving in water-bath, lead to nitrogen
Gas is drained air, adds initiator to cause, adds acrylamide and obtain reactant liquor, react rear product and be cooled to room temperature, washs,
Dry in vacuum drying chamber, obtain crude product；
(2) preparation of smart product：Step (1) gained crude product is put into acetic acid and immersion in ethylene glycol mixture, then is put
Dry in vacuum drying chamber, obtain paper making intensifier of the smart product i.e. based on hemicellulose.
Preferably, the temperature of step (1) water-bath is 40 DEG C～80 DEG C.
Preferably, step (1) initiator is potassium peroxydisulfate, initiator and xylan mass ratio 1 for initiator:(2～
13)；The time of the initiation is 10min.It is further preferred that the consumption of the initiator is 0.0003～0.0017mol.
Preferably, step (1) the xylan powder is 1 with the mass ratio of acrylamide：(1～4).
It is further preferred that the quality of step (1) the xylan powder is 1g.
Preferably, concentration of the acrylamide in step (1) gained reactant liquor is 0.176mol/L～1.057mol/L；Enter
One step is preferred, and the concentration of acrylamide is 0.354mol/L.
Preferably, in step (1), xylan is 40 DEG C～80 DEG C with the temperature of acrylamide reaction, and the time is 2h～6h；
It is further preferred that the temperature of reaction is 60 DEG C, the time of reaction is 4h..
Preferably, step (1) the xylan modification prepares the concrete conduct of xylan grafted polyacrylamide：Wood is poly-
It is stirring and dissolving 30min in 60 DEG C of hot water that sugar adds temperature, is subsequently adding initiator potassium persulfate, adds certain after 10min
Amount acrylamide, reacts 2h～6h, wherein xylan at 60 DEG C：The proportion of acylamide is 1：(1～4).
Preferably, step (2) acetic acid is 4 with the volume ratio of acetic acid in ethylene glycol mixture and ethylene glycol:6～8:
2.
Preferably, the number of times of step (2) immersion is 3～5 times, and the time that soaks every time is 2～3h.
Preferably, step (1), step (2) drying be in 40 DEG C～80 DEG C 12～24h of drying.
The present invention also provides a kind of paper making intensifier based on hemicellulose obtained in above-described preparation method.Should
Can apply in paper industry based on the paper making intensifier of hemicellulose.
Compared with prior art, the invention has the advantages that and beneficial effect：
(1) xylan grafted polyacrylamide prepared by the present invention, the characteristic with polyacrylamide, while also have wood
The performance of glycan, can be applied to paper industry as paper making intensifier.
(2), during xylan grafted polyacrylamide prepared by the present invention, reaction condition is gentle, easy controlled operation, easily
In realization industrialization.
Description of the drawings
Fig. 1 is the infared spectrum of xylan and xylan grafted polyacrylamide in embodiment 1.
Specific embodiment
Below in conjunction with implementing to be further explained the present invention explanation, but embodiments of the present invention not limited to this.
Embodiment 1
(1) the xylan powder for weighing 1g is dissolved in ultra-pure water, heating for dissolving in 60 DEG C of water-baths, and logical nitrogen is drained air,
0.0003mol initiator potassium persulfate is added, the acrylamide monomer of 1g after 10min, is added, 2h is reacted at 60 DEG C.
(2) product of step (1) is cooled to room temperature, is washed with acetone, filter 23 time, by the product for filtering logical
After wind cupboard places 3h, be put in vacuum drying chamber, 12h dry at 40 DEG C, obtain crude product.
(3) crude product for drying step (2) is put into acetic acid and ethylene glycol mixture (acetic acid with the volume ratio of ethylene glycol is
4:6) soak 3 times in, each 2h, after 3h placed by fume hood, be put in vacuum drying chamber, at 60 DEG C, 24h dry, obtain smart product
Product are xylan grafted polyacrylamide.
The product graft rate for obtaining is 27.02%, and the xylan graft acrylamide that 0.054g mass fraction is 1% is added
Dense for 0.5wt% pulp from ONP to slurry, test through handsheet and after 24h places in thermostatic constant wet chamber, test through paper performance,
Former pulp strength is as follows：Burst index is 1.5Kpa m2/g, and tear index is 6.02mN m2/g, and tensile strength is
1.21kN/m.26.4% is improve with respect to its tensile strength of intensity of body paper slurry, tear index improves 30.2%, and bursting strength is carried
High by 20.3%, folding strength number of times improves obvious.There is to pulp property one significantly to improve, have in paper industry application
There is very big prospect.
Embodiment 2
(1) the xylan powder for weighing 1g is dissolved in ultra-pure water, heating for dissolving in 60 DEG C of water-baths, and logical nitrogen is drained air,
0.001mol initiator potassium persulfate is added, the acrylamide monomer of 2g after 10min, is added, 4h is reacted at 70 DEG C.
(2) product of step (1) is cooled to room temperature, is washed with acetone, filter 23 time, by the product for filtering logical
After wind cupboard places 3h, be put in vacuum drying chamber, 24h dry at 60 DEG C, obtain crude product.
(3) crude product for drying step (2) is put into acetic acid and ethylene glycol mixture (acetic acid with the volume ratio of ethylene glycol is
6:4) soak 4 times in, each 2.5h, after 3h placed by fume hood, be put in vacuum drying chamber, 24h dry at 60 DEG C, obtain
Smart product is xylan grafted polyacrylamide.
The product graft rate for obtaining is 84.96%, and the xylan graft acrylamide that 0.054g mass fraction is 1% is added
Dense for 0.5wt% pulp from ONP to slurry, test through handsheet and after 24h places in thermostatic constant wet chamber, test through paper performance,
Former pulp strength is as follows：Burst index is 1.5Kpa m2/g, and tear index is 6.02mN m2/g, and tensile strength is
1.21kN/m.27.3% is improve with respect to its tensile strength of intensity of body paper slurry, tear index improves 49.2%, and bursting strength is carried
High by 24.5%, folding strength number of times improves obvious.There is to pulp property one significantly to improve, have in paper industry application
There is very big prospect.
Embodiment 3
(1) the xylan powder for weighing 1g is dissolved in ultra-pure water, heating for dissolving in 60 DEG C of water-baths, and logical nitrogen is drained air,
0.0017mol initiator potassium persulfate is added, the acrylamide monomer of 4g after 10min, is added, 6h is reacted at 80 DEG C.
(2) product of step (1) is cooled to room temperature, is washed with acetone, filter 23 time, by the product for filtering logical
After wind cupboard places 3h, be put in vacuum drying chamber, 24h dry at 60 DEG C, obtain crude product.
(3) crude product for drying step (2) is put into acetic acid and ethylene glycol mixture (acetic acid with the volume ratio of ethylene glycol is
8:2) soak 5 times in, each 3h, after 3h placed by fume hood, be put in vacuum drying chamber, 24h dry at 60 DEG C, obtain essence
Product is xylan grafted polyacrylamide.
The product graft rate for obtaining is 35.44%, and the xylan graft acrylamide that 0.054g mass fraction is 1% is added
Dense for 0.5wt% pulp from ONP to slurry, test through handsheet and after 24h places in thermostatic constant wet chamber, test through paper performance,
Former pulp strength is as follows：Burst index is 1.5Kpa m2/g, and tear index is 6.02mN m2/g, and tensile strength is
1.21kN/m.31.4% is improve with respect to its tensile strength of intensity of body paper slurry, tear index improves 24.9%, and bursting strength is carried
High by 23.3%, folding strength number of times improves obvious.There is to pulp property one significantly to improve, have in paper industry application
There is very big prospect.
It can be seen from figure 1 that flexible the shaking of the xylan of embodiment 1 and xylan grafted polyacrylamide Jun You functional group O-H
Move in 3600～3200cm-1There is a broad peak；The stretching vibration of C-H is in 3000～2800cm-1There is a broad peak；Carbon water
The stretching vibration of compound C=O is in 1665～1600cm-1There is a broad peak；The stretching vibration of C-O is in 1200～1000cm-1There are 2 broad peaks.The infrared spectrogram of contrast xylan, the infrared spectrogram of xylan grafted polyacrylamide, 3600～
3200cm-1Absworption peak obvious, this is-OH and-NH2Being overlapped mutually for absworption peak of stretching vibration and produce
,-NH2Stretching vibration absworption peak, can be superimposed due to hydroxyl absorption peak wide by force, can only see an acromion.1100
～1300cm-1The absworption peak of C-N is occurred in that, these are all the due absworption peaks of polyacrylamide, xylan in other embodiments
And the infared spectrum of xylan grafted polyacrylamide is consistent with Fig. 1, xylan graft polypropylene acyl prepared by the present invention is described
Amine, the characteristic with polyacrylamide, while also having the performance of xylan, paper maker can be applied to as paper making intensifier
Industry.
The elementary analysis of xylan and xylan grafted polyacrylamide is as shown in table 1.
Table 1
As seen from Table 1, the mass fraction of the N of xylan graft copolymer increases substantially, can obtain graft copolymer increasing
Add in the conclusion of the functional group of N, i.e. graft copolymer and connected PAM.And as percent grafting increases, the content of N continues to increase.
Containing S, graft copolymer is that initiator does not have fully erased clean.
Claims (10)
1. a kind of preparation method of the paper making intensifier based on hemicellulose, it is characterised in that comprise the steps：
（1）Xylan graft copolymerization：Weigh xylan powder to be dissolved in ultra-pure water, heating for dissolving in water-bath, lead to nitrogen row
Fall air, add initiator to cause, add acrylamide and reactant liquor is obtained, reacted rear product and room temperature is cooled to, washing, true
Dry in empty drying box, obtain crude product；
（2）The preparation of smart product：By step（1）Gained crude product is put into acetic acid and immersion in ethylene glycol mixture, then is put into true
Dry in empty drying box, obtain paper making intensifier of the smart product i.e. based on hemicellulose.
2. preparation method according to claim 1, it is characterised in that step（1）The temperature of the water-bath is 40 DEG C～80
℃.
3. preparation method according to claim 1, it is characterised in that step（1）The initiator is potassium peroxydisulfate, causes
Agent is 1 with the mass ratio of xylan powder:(2～13)；The time of the initiation is 10min.
4. preparation method according to claim 1, it is characterised in that step（1）The xylan powder and acrylamide
Mass ratio be 1：（1～4）；Acrylamide is in step（1）Concentration in gained reactant liquor is 0.176mol/L～1.057
mol/L.
5. preparation method according to claim 1, it is characterised in that step（1）Middle xylan and acrylamide reaction
Temperature is 40 DEG C～80 DEG C, and the time is 2h～6h.
6. preparation method according to claim 1, it is characterised in that step（2）In the acetic acid and ethylene glycol mixture
Acetic acid is 4 with the volume ratio of ethylene glycol:6～8:2.
7. preparation method according to claim 1, it is characterised in that step（2）The number of times of the immersion is 3～5 times, per
The time of secondary immersion is 2～3h.
8. preparation method according to claim 1, it is characterised in that step（1）, step（2）The drying be 40oC～
80oC dries 12～24h.
9. a kind of paper making intensifier based on hemicellulose obtained in the preparation method described in any one of claim 1-8.
10. a kind of paper making intensifier based on hemicellulose described in claim 9 is applied in papermaking.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109653025A (en) * | 2018-12-12 | 2019-04-19 | 济宁明升新材料有限公司 | A kind of preparation method of natural polysaccharide and its derivative modified wet strengthening agents for papermaking |
| CN112619322A (en) * | 2021-01-15 | 2021-04-09 | 王忠良 | Air filtering membrane replacing melt-blown fabric and preparation method thereof |
| CN112741731A (en) * | 2021-01-15 | 2021-05-04 | 王忠良 | Paper diaper absorbing core layer and production process thereof |
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| CN101962424A (en) * | 2010-09-16 | 2011-02-02 | 桂林理工大学 | Preparation method of acrylamide/methyl methacrylate grafted bagasse xylan copolymer |
| CN103214598A (en) * | 2013-04-25 | 2013-07-24 | 华南理工大学 | Quaternization xylan, preparation method via semi-dry process and application of quaternization xylan |
| CN103889395A (en) * | 2011-11-04 | 2014-06-25 | 阿克佐诺贝尔化学国际公司 | Graft dendrite copolymers, and methods for producing the same |
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| CN101962424A (en) * | 2010-09-16 | 2011-02-02 | 桂林理工大学 | Preparation method of acrylamide/methyl methacrylate grafted bagasse xylan copolymer |
| CN103889395A (en) * | 2011-11-04 | 2014-06-25 | 阿克佐诺贝尔化学国际公司 | Graft dendrite copolymers, and methods for producing the same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109653025A (en) * | 2018-12-12 | 2019-04-19 | 济宁明升新材料有限公司 | A kind of preparation method of natural polysaccharide and its derivative modified wet strengthening agents for papermaking |
| CN112619322A (en) * | 2021-01-15 | 2021-04-09 | 王忠良 | Air filtering membrane replacing melt-blown fabric and preparation method thereof |
| CN112741731A (en) * | 2021-01-15 | 2021-05-04 | 王忠良 | Paper diaper absorbing core layer and production process thereof |
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| CN106480780B (en) | 2018-06-22 |
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