CN106480780B - 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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- CN106480780B CN106480780B CN201610939162.0A CN201610939162A CN106480780B CN 106480780 B CN106480780 B CN 106480780B CN 201610939162 A CN201610939162 A CN 201610939162A CN 106480780 B CN106480780 B CN 106480780B
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- xylan
- preparation
- 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
-
- 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
Abstract
The invention discloses a kind of paper making intensifiers based on hemicellulose and preparation method and application.This method includes the following steps：Xylan is dissolved in ultra-pure water, is dissolved by heating in water-bath, leads to nitrogen, adds in initiator, causes and adds in grafted monomers acrylamide after a certain period of time, product cooling, is washed with acetone after having reacted, and then vacuum drying obtains crude product.Dry crude product is put into acetic acid with being impregnated in ethylene glycol mixture repeatedly, then vacuum drying obtains the high xylan grafted polyacrylamide of purity.The xylan grafted polyacrylamide has both xylan and polyacrylamide performance, and price is less expensive, flocculability is good, effectively improves the paper performance of secondary stock.The preparation method of the present invention has technique characteristic easy to operate, environmental-friendly.
Description
Technical field
The present invention relates to paper making intensifier fields, and in particular to a kind of paper making intensifier and its preparation based on hemicellulose
Method and application.
Background technology
Due to gradually exhausted and environmental problem the continuous deterioration of fossil resource.Agricultural-forestry biomass have it is environmental-friendly, can
Biodegradable, the advantages that regeneration period is short.Being prepared using agricultural wastes, there are high valuable chemicals to be considered as solving environment
And one of effective way of energy problem.
Xylan grafted polyacrylamide is the derivative of xylan after being chemically modified, by xylan and acrylamide
High temperature graft copolymerization is made, and has the strong flocculability of polyacrylamide, has very strong flocculating effect to the solute in solution, and poly-
There are amide groups for acrylamide, can form hydrogen bond with cellulose, size performance effectively be improved, therefore can be applied to make
Paper industry.Xylan grafted polyacrylamide prepared by this method has environment friendly, and environmental pollution is small.
In recent years, the deep processing of biomass receives the graft copolymerization of the concern of many scientific workers, wherein biomass
Method of modifying is particularly noticeable.Biomass graft copolymerization includes, the graft copolymerization of cellulose, the graft copolymerization of hemicellulose,
Graft copolymerization of chitosan etc..Biomass after grafting, copolymerization and modification has the superperformance of grafted monomers, makes biomass
Application range is more extensive, becomes the hot spot studied both at home and abroad.Traditional papermaking is replaced to enhance using xylan graft acrylamide
The shortcomings of agent greatly reduces production cost, environmental pollution has technology and feasibility economically.
Invention content
In order to solve the disadvantage that the more than prior art and shortcoming, the purpose of the present invention is to provide one kind to be based on half fiber
Tie up paper making intensifier of element and preparation method and application.The xylan grafted polyacrylamide has both xylan and polyacrylamide
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
It is 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, includes the following steps：
(1) xylan graft copolymerization：It weighs xylan powder to be dissolved in ultra-pure water, be dissolved by heating in water-bath, lead to nitrogen
Gas exhausts air, adds in initiator and causes, adds acrylamide and obtain reaction solution, and product is cooled to room temperature after having reacted, and is washed,
It is dry in vacuum drying chamber, obtain crude product；
(2) preparation of smart product：Crude product obtained by step (1) is put into acetic acid with being impregnated in ethylene glycol mixture, then put
It is dry into vacuum drying chamber, obtain the smart product i.e. paper making intensifier based on hemicellulose.
Preferably, the temperature of step (1) described water-bath is 40 DEG C~80 DEG C.
Preferably, it is potassium peroxydisulfate, initiator and xylan mass ratio 1 that step (1) described initiator, which is initiator,:(2~
13)；The time of the initiation is 10min.It is further preferred that the dosage of the initiator is 0.0003~0.0017mol.
Preferably, the mass ratio of step (1) the xylan powder and acrylamide is 1：(1~4).
It is further preferred that the quality of step (1) the xylan powder is 1g.
Preferably, a concentration of 0.176mol/L~1.057mol/L of the acrylamide in reaction solution obtained by step (1)；Into
One step is preferred, a concentration of 0.354mol/L of acrylamide.
Preferably, the temperature that xylan is reacted with acrylamide in step (1) is 40 DEG C~80 DEG C, 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 specific conduct of xylan grafted polyacrylamide：Wood is poly-
Sugar is added in the hot water that temperature is 60 DEG C, stirring and dissolving 30min, is then added in initiator potassium persulfate, is added in after 10min certain
Acrylamide is measured, reacts 2h~6h, wherein xylan at 60 DEG C：The proportion of acylamide is 1：(1~4).
Preferably, step (2) acetic acid and the volume ratio of acetic acid and ethylene glycol in ethylene glycol mixture are 4:6~8:
2。
Preferably, the number of step (2) described immersion is 3~5 times, and the time impregnated every time is 2~3h.
Preferably, step (1), step (2) described drying are in 40 DEG C~80 DEG C dryings 12~for 24 hours.
The present invention also provides the paper making intensifiers based on hemicellulose a kind of as made from above-described preparation method.It should
Paper making intensifier based on hemicellulose can apply in paper industry.
Compared with prior art, the invention has the advantages that and advantageous effect：
(1) xylan grafted polyacrylamide prepared by the present invention has the characteristic of polyacrylamide, while also has wood
The performance of glycan can be used as paper making intensifier to be applied to paper industry.
(2) during xylan grafted polyacrylamide prepared by the present invention, reaction condition is mild, easy controlled operation, easily
It is industrialized in realizing.
Description of the drawings
Fig. 1 is the infared spectrum of xylan and xylan grafted polyacrylamide in embodiment 1.
Specific embodiment
Explanation is further explained to the present invention, but the implementation of the present invention is not limited to this below in conjunction with implementation.
Embodiment 1
(1) the xylan powder for weighing 1g is dissolved in ultra-pure water, is dissolved by heating in 60 DEG C of water-baths, and logical nitrogen exhausts air,
0.0003mol initiator potassium persulfates are added in, the acrylamide monomer of 1g is added in after 10min, react 2h at 60 DEG C.
(2) reaction product of step (1) is cooled to room temperature, is washed with acetone, filter 23, by the product of filtering logical
It after wind cupboard places 3h, is put into vacuum drying chamber, dry 12h, obtains crude product at 40 DEG C.
(3) the dry crude product of step (2) is put into acetic acid and ethylene glycol mixture (volume ratio of acetic acid and ethylene glycol is
4:6) it impregnates 3 times, each 2h in, after draught cupboard places 3h, is put into vacuum drying chamber, dried for 24 hours at 60 DEG C, obtain smart production
Product, that is, xylan grafted polyacrylamide.
Obtained product graft rate is 27.02%, and the xylan graft acrylamide that 0.054g mass fractions are 1% is added
It is 0.5wt% pulp from ONP to starching dense, tests through handsheet and after thermostatic constant wet chamber places for 24 hours, tested through paper performance,
Former pulp strength is as follows：Burst index is 1.5Kpam2/g, tear index 6.02mNm2/g, and tensile strength is
1.21kN/m.With respect to the intensity of body paper slurry, its tensile strength improves 26.4%, and tear index improves 30.2%, and bursting strength carries
High by 20.3%, folding strength number improves obvious.Pulp property there are one apparent is improved, is had in paper industry application
There is very big prospect.
Embodiment 2
(1) the xylan powder for weighing 1g is dissolved in ultra-pure water, is dissolved by heating in 60 DEG C of water-baths, and logical nitrogen exhausts air,
0.001mol initiator potassium persulfates are added in, the acrylamide monomer of 2g is added in after 10min, react 4h at 70 DEG C.
(2) reaction product of step (1) is cooled to room temperature, is washed with acetone, filter 23, by the product of filtering logical
It after wind cupboard places 3h, is put into vacuum drying chamber, is dried for 24 hours at 60 DEG C, obtain crude product.
(3) the dry crude product of step (2) is put into acetic acid and ethylene glycol mixture (volume ratio of acetic acid and ethylene glycol is
6:4) it impregnates 4 times, each 2.5h in, after draught cupboard places 3h, is put into vacuum drying chamber, dry for 24 hours, obtain at 60 DEG C
Smart product, that is, xylan grafted polyacrylamide.
Obtained product graft rate is 84.96%, and the xylan graft acrylamide that 0.054g mass fractions are 1% is added
It is 0.5wt% pulp from ONP to starching dense, tests through handsheet and after thermostatic constant wet chamber places for 24 hours, tested through paper performance,
Former pulp strength is as follows：Burst index is 1.5Kpam2/g, tear index 6.02mNm2/g, and tensile strength is
1.21kN/m.With respect to the intensity of body paper slurry, its tensile strength improves 27.3%, and tear index improves 49.2%, and bursting strength carries
High by 24.5%, folding strength number improves obvious.Pulp property there are one apparent is improved, is had in paper industry application
There is very big prospect.
Embodiment 3
(1) the xylan powder for weighing 1g is dissolved in ultra-pure water, is dissolved by heating in 60 DEG C of water-baths, and logical nitrogen exhausts air,
0.0017mol initiator potassium persulfates are added in, the acrylamide monomer of 4g is added in after 10min, react 6h at 80 DEG C.
(2) reaction product of step (1) is cooled to room temperature, is washed with acetone, filter 23, by the product of filtering logical
It after wind cupboard places 3h, is put into vacuum drying chamber, is dried for 24 hours at 60 DEG C, obtain crude product.
(3) the dry crude product of step (2) is put into acetic acid and ethylene glycol mixture (volume ratio of acetic acid and ethylene glycol is
8:2) it impregnates 5 times, each 3h in, after draught cupboard places 3h, is put into vacuum drying chamber, dried for 24 hours at 60 DEG C, obtain essence
Product, that is, xylan grafted polyacrylamide.
Obtained product graft rate is 35.44%, and the xylan graft acrylamide that 0.054g mass fractions are 1% is added
It is 0.5wt% pulp from ONP to starching dense, tests through handsheet and after thermostatic constant wet chamber places for 24 hours, tested through paper performance,
Former pulp strength is as follows：Burst index is 1.5Kpam2/g, tear index 6.02mNm2/g, and tensile strength is
1.21kN/m.With respect to the intensity of body paper slurry, its tensile strength improves 31.4%, and tear index improves 24.9%, and bursting strength carries
High by 23.3%, folding strength number improves obvious.Pulp property there are one apparent is improved, is had in paper industry application
There is very big prospect.
It can be seen from figure 1 that flexible the shaking of the xylan and xylan grafted polyacrylamide Jun You functional group O-H of embodiment 1
It moves 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 comparison xylan, the infrared spectrogram of xylan grafted polyacrylamide, 3600~
3200cm-1Absorption peak it is obvious, this is-OH and-NH2Stretching vibration being overlapped mutually for absorption peak and generate
,-NH2Stretching vibration absorption peak, can be superimposed due to strong wide hydroxyl absorption peak, can only see an acromion.1100
~1300cm-1There is the absorption peak of C-N, these are all the due absorption peaks of polyacrylamide, xylan in other embodiments
And the infared spectrum of xylan grafted polyacrylamide is consistent with Fig. 1, illustrates xylan graft polypropylene acyl prepared by the present invention
Amine has the characteristic of polyacrylamide, while also has the performance of xylan, paper making intensifier can be used as to be applied to paper maker
Industry.
The elemental 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 apparent, can obtain graft copolymer increasing
Add the conclusion of the functional group of N, i.e., connect PAM in graft copolymer.And as grafting rate increases, the content of N continues to increase.
It is fully erased clean that graft copolymer containing S is that initiator does not have.
Claims (9)
1. a kind of preparation method of the paper making intensifier based on hemicellulose, which is characterized in that include the following steps：
（1）Xylan graft copolymerization：It weighs xylan powder to be dissolved in ultra-pure water, be dissolved by heating in water-bath, lead to nitrogen row
Fall air, add in initiator and cause, add acrylamide and obtain reaction solution, product is cooled to room temperature after having reacted, and is washed, true
It is dry in empty drying box, obtain crude product；The temperature of the water-bath is 40 DEG C~80 DEG C；
（2）The preparation of smart product：By step（1）Gained crude product is put into acetic acid and is impregnated in ethylene glycol mixture, then is put into true
It is dry in empty drying box, obtain the smart product i.e. paper making intensifier based on hemicellulose.
2. preparation method according to claim 1, which is characterized in that step（1）The initiator is potassium peroxydisulfate, is caused
The mass ratio of agent and xylan powder is 1:(2~13)；The time of the initiation is 10min.
3. preparation method according to claim 1, which is characterized in that step（1）The xylan powder and acrylamide
Mass ratio be 1：（1~4）；Acrylamide is in step（1）A concentration of 0.176mol/L~1.057 in gained reaction solution
mol/L。
4. preparation method according to claim 1, which is characterized in that step（1）What middle xylan was reacted with acrylamide
Temperature is 40 DEG C~80 DEG C, and the time is 2h~6h.
5. preparation method according to claim 1, which is characterized in that step（2）In the acetic acid and ethylene glycol mixture
The volume ratio of acetic acid and ethylene glycol is 4:6~8:2.
6. preparation method according to claim 1, which is characterized in that step（2）The number of the immersion is 3~5 times, often
The time of secondary immersion is 2~3h.
7. preparation method according to claim 1, which is characterized in that step（1）, step（2）The drying is 40oC~
80oC dryings 12~for 24 hours.
8. a kind of paper making intensifier based on hemicellulose as made from claim 1-7 any one of them preparation methods.
9. a kind of paper making intensifier based on hemicellulose according to any one of claims 8 is applied in paper industry.
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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 |
| CN112741731A (en) * | 2021-01-15 | 2021-05-04 | 王忠良 | Paper diaper absorbing core layer and production process thereof |
| CN112619322A (en) * | 2021-01-15 | 2021-04-09 | 王忠良 | Air filtering membrane replacing melt-blown fabric and preparation method 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 |
| 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 |
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