CN101870748A - Preparation and application methods of polyacrylic acid amide modifier for fly ash fiber paper making - Google Patents
Preparation and application methods of polyacrylic acid amide modifier for fly ash fiber paper making Download PDFInfo
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- CN101870748A CN101870748A CN 201010202753 CN201010202753A CN101870748A CN 101870748 A CN101870748 A CN 101870748A CN 201010202753 CN201010202753 CN 201010202753 CN 201010202753 A CN201010202753 A CN 201010202753A CN 101870748 A CN101870748 A CN 101870748A
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- polyacrylic acid
- acid amide
- ash fiber
- coal ash
- fly ash
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Abstract
The invention relates to preparation and application methods of polyacrylic acid amide modifier for fly ash fiber paper making, which are characterized in: first, polymerizing acrylic acid in water phase into polyacrylic acid, and then adding , N-dimethyl-1,3-propanediamine into polyacrylic acid solution to be amidated; increasing the temperature of an obtained amidation product to 50 to 80DEG C, adding in bromo-n-butane for quaterisation to obtain the polyacrylic acid amide modifier; dispersing fly ash fibers into water, adding in the polyacrylic acid amide modifier, stirring for 10 to 15min, adding in wood fiber pulp, uniformly mixing, making paper on a paper forming machine to obtain the paper containing fly ash fibers. The polyacrylic acid amide modifier prepared through the method can enhance the bonding force between the fly ash fibers and wood pulp fibers so as to improve the strength of the paper containing fly ash fibers.
Description
Technical field
The present invention relates to a kind of coal ash fiber of papermaking and the preparation and application method thereof of xylon mixed dissolving modifier of being used for.
Background technology
A large amount of hydroxyls and small number of carboxylic acid groups are contained in the wood pulp cellulose surface, and these hydroxyls can make fiber disperse better in water, also can the combination by the hydrogen bond force between hydroxyl between the fiber.Coal ash fiber is white or lurid floss, is raw material with flyash, a kind of novel inorganic fibre of making through operations such as high temperature melting, spray silk, coolings.Its main component is SiO
2, Al
2O
3, CaO, Fe
2O
3The surface of fly ash fiber smoother, hydroxy radical content is far smaller than wood pulp cellulose.This directly cause between coal ash fiber self and and wood pulp cellulose between bonding force poor, have influence on the application of coal ash fiber aspect papermaking.So improve the emphasis that is combined into research between coal ash fiber and the wood pulp cellulose.
Chinese patent CN101654891A discloses the new process of production of the efficient paper-making dispersant agent of a kind of acrylic amide, and pure water, yellow soda ash, sodium bicarbonate, tensio-active agent, function monomer, functional agent are modulated.The polymerization of gained modulating liquid is got jel product.Final product is grade packaged through granulation, drying, grinding, branch, required paper-making fibre dispersion agent.This invention is applicable to paper-making fibre and disperses.The gained dispersion agent has that dispersion effect is good, molecular weight is high, good water solubility, non-toxic efficient, advantage such as cheap.
Chinese patent CN101666056A discloses a kind of fly-ash mine fiber paper pulp and preparation technology thereof.Its concrete technology is: with slag, silica and coke mixing granulation on request, burnt material is than being defined as between the 0.12-0.23, with the said mixture high temperature melting, its melt gets rid of silk through whizzer and forms the ore deposit fiber, and the ore deposit fiber dispersion obtains fly-ash mine fiber paper pulp after softening, remove the gred, concentrate, copy the slurry dehydration then.The fine slurry in the ore deposit of this prepared is applicable to papermaking, thereby the alternative or alternative papermaking wood pulp of part is saved the log loss, protects forest resources, and reduces by 20% cost than organic plant fiber papermaking, and manufacture craft is simple, the making processes environmental protection.
Chinese patent CN1580391A discloses a kind of fly ash fiber pulp and has been the papermaking side of raw material.Its technical scheme is: tenderizer 1～10%, dispersion agent 1～8%, surface-modifying agent 1～10%, coal ash fiber 20～80%, organic fibre, water are deployed into flyash paper pulp.The gained paper physical property reaches the equal performance of vegetable fibre paper, is being better than the vegetable fibre paper aspect water tolerance, anti-protection against corrosion and the fire line.This invention can reduce the papermaking cost, gives industrial waste with the functionalization utilization, replaces wood pulp, saves log and expends, and is remarkable to the meaning that protects forest resources.
Above-described invention has certain help for coal ash fiber papermaking, but can not improve the binding ability of coal ash fiber and wood pulp cellulose at all.The present invention seeks to increases the binding ability of coal ash fiber and xylon from both binding abilities of origin solution by adding a kind of properties-correcting agent.The innovative approach of head it off of the present invention is: synthetic a kind ofly be skeleton, introduce the properties-correcting agent of positive ion or cation group on its chain with the water-soluble polymers polyacrylic acid.Surface of fly ash fiber is electronegative, properties-correcting agent with positive charge can be by electrostatic force and coal ash fiber combination, with negative charge can make the modifier molecules chain-unfolding, thereby evenly adhere at fiber surface, institute's synthetic properties-correcting agent has the part amido linkage again, and this part can be by a large amount of hydroxyl combination on hydrogen bond action power and the xylon.And institute's synthetic properties-correcting agent can obtain the different properties-correcting agent of zwitterion proportioning by changing electrochemical conditions, can test motive power the size of the degree influence of keying action is adjusted its zwitterion proportioning, obtains best electric charge ratio.
Summary of the invention
A kind of preparation of polyacrylic acid amide modifier for fly ash fiber paper making and application method, it is characterized in that: at aqueous phase acroleic acid polymerization is become polyacrylic acid earlier, again with N, N-dimethyl-1, the 3-propylene diamine joins and carries out amidation in the polyacrylic acid aqueous solution, the gained amidated products is warming up to 50～80 ℃, and the adding bromination of n-butane carries out quaternized, obtains polyacrylic acid amide modifier.Then, coal ash fiber is dispersed in the water, adds polyacrylic acid amide modifier, stirred 10～15 minutes, interpolation xylon slurry, after mixing, papermaking on the sheet forming machine obtains containing the paper of coal ash fiber.
Described acroleic acid polymerization method is: add earlier the ammonium persulphate of entry, sodium bisulfite, ammonium persulphate gross weight 15%, the vinylformic acid of vinylformic acid gross weight 15% in reactor, the add-on of sodium bisulfite is 2%～8% of a vinylformic acid oven dry weight, reactor is warming up to 70 ℃, remains 85% vinylformic acid then and be made into the aqueous solution and 85% ammonium persulphate and be made into the aqueous solution and be added drop-wise in the reactor simultaneously.Total add-on of ammonium persulphate is 1%～4% of a vinylformic acid oven dry weight, and the dropping time is 2～3 hours.After dropwising, be warming up to 90～92 ℃, be incubated 3 hours, be cooled to below 40 ℃.
Described N, N-dimethyl-1, the add-on of 3-propylene diamine is: vinylformic acid and N, N-dimethyl-1, the molar ratio of 3-propylene diamine are 1: 1～3: 1.
The add-on of described bromination of n-butane is: bromination of n-butane and acrylic acid molar ratio are 1: 1.
Described at coal ash fiber aqueous phase adding polyacrylic acid amide modifier, its add-on is: in the oven dry weight polyacrylic acid amide modifier is 1～10% of coal ash fiber.
Described coal ash fiber and xylon, in dry pulp weight coal ash fiber: wood pulp cellulose is 1: 2.
Embodiment
Embodiment 1
The ammonium persulphate that in the reactor that 250 milliliters of bands stir, heat, adds 80g water, 3g vinylformic acid, 0.4g sodium bisulfite, 0.03g, opening to stir fully dissolves it, reacting by heating still to temperature rises to 70 ℃, again 17g vinylformic acid is made into 50% the aqueous solution, 0.17g ammonium persulphate and is made into 5% the aqueous solution, splash in the reactor simultaneously.The dropping time is 2 hours, is warming up to 90 ℃ then, is incubated 3 hours, is cooled to 40 ℃, obtains the 120.8g polyacrylic acid aqueous solution.In the polyacrylic acid aqueous solution, add N again, N-dimethyl-1,3-propylene diamine 56g carries out amidation, is warming up to 50 ℃, adds bromination of n-butane 38g then, gets polyacrylic acid amide properties-correcting agent 214.8g.
The 9g coal ash fiber is dispersed in the 3000ml water, soaked 20 minutes, add the 0.09g polyacrylic acid amide modifier, stirred 10 minutes, and added the 18g wood pulp cellulose again, stirred 5 minutes, stop to stir, papermaking on the sheet forming machine then obtains containing the paper of coal ash fiber.
Embodiment 2
The ammonium persulphate that in the reactor that 250 milliliters of bands stir, heat, adds 80g water, 3g vinylformic acid, 0.8g sodium bisulfite, 0.06g, opening to stir fully dissolves it, reacting by heating still to temperature rises to 70 ℃, again 17g vinylformic acid is made into 50% the aqueous solution, 0.34g ammonium persulphate and is made into 10% the aqueous solution, splash in the reactor simultaneously.The dropping time is 2 hours, is warming up to 90 ℃ then, is incubated 3 hours, is cooled to 40 ℃, obtains the 212.2g polyacrylic acid aqueous solution.In the polyacrylic acid aqueous solution, add N again, N-dimethyl-1,3-propylene diamine 85g carries out amidation, is warming up to 80 ℃, adds bromination of n-butane 38g then, gets polyacrylic acid amide properties-correcting agent 244.2g.
The 9g coal ash fiber is dispersed in the 3000ml water, soaked 20 minutes, add the 0.9g polyacrylic acid amide modifier, stirred 15 minutes, and added the 18g wood pulp cellulose again, stirred 5 minutes, stop to stir, papermaking on the sheet forming machine then obtains containing the paper of coal ash fiber.
Embodiment 3
The ammonium persulphate that in the reactor that 250 milliliters of bands stir, heat, adds 80g water, 3g vinylformic acid, 1.2g sodium bisulfite, 0.09g, opening to stir fully dissolves it, reacting by heating still to temperature rises to 70 ℃, again 17g vinylformic acid is made into 50% the aqueous solution, 0.51g ammonium persulphate and is made into 10% the aqueous solution, splash in the reactor simultaneously.The dropping time is 2 hours, is warming up to 90 ℃ then, is incubated 3 hours, is cooled to 40 ℃, obtains the 123.3g polyacrylic acid aqueous solution.In the polyacrylic acid aqueous solution, add N again, N-dimethyl-1,3-propylene diamine 28g carries out amidation, is warming up to 70 ℃, adds bromination of n-butane 38g then, gets polyacrylic acid amide properties-correcting agent 189.3g.
The 9g coal ash fiber is dispersed in the 3000ml water, soaked 20 minutes, add the 0.15g polyacrylic acid amide modifier, stirred 12 minutes, and added the 18g wood pulp cellulose again, stirred 5 minutes, stop to stir, papermaking on the sheet forming machine then obtains containing the paper of coal ash fiber.
Embodiment 4
The ammonium persulphate that in the reactor that 250 milliliters of bands stir, heat, adds 80g water, 3g vinylformic acid, 1.6g sodium bisulfite, 0.12g, opening to stir fully dissolves it, reacting by heating still to temperature rises to 70 ℃, again 17g vinylformic acid is made into 50% the aqueous solution, 0.60g ammonium persulphate and is made into 10% the aqueous solution, splash in the reactor simultaneously.The dropping time is 2 hours, is warming up to 90 ℃ then, is incubated 3 hours, cools off 40 ℃, obtains the 124.7g polyacrylic acid aqueous solution.In the polyacrylic acid aqueous solution, add N again, N-dimethyl-1,3-propylene diamine 70g carries out amidation, is warming up to 60 ℃, adds bromination of n-butane 38g then, gets polyacrylic acid amide properties-correcting agent 232.7g.
The 9g coal ash fiber is dispersed in the 3000ml water, soaked 20 minutes, add the 0.6g polyacrylic acid amide modifier, stirred 14 minutes, and added the 18g wood pulp cellulose again, stirred 5 minutes, stop to stir, papermaking on the sheet forming machine then obtains containing the paper of coal ash fiber.
Embodiment 5
The ammonium persulphate that in the reactor that 250 milliliters of bands stir, heat, adds 80g water, 3g vinylformic acid, 0.8g sodium bisulfite, 0.06g, opening to stir fully dissolves it, reacting by heating still to temperature rises to 70 ℃, again 17g vinylformic acid is made into 50% the aqueous solution, 0.34g ammonium persulphate and is made into 10% the aqueous solution, splash in the reactor simultaneously.The dropping time is 2 hours, is warming up to 90 ℃ then, is incubated 3 hours, cools off 40 ℃, obtains the 121.2g polyacrylic acid aqueous solution.In the polyacrylic acid aqueous solution, add N again, N-dimethyl-1,3-propylene diamine 42g carries out amidation, is warming up to 75 ℃, adds bromination of n-butane 38g then, gets polyacrylic acid amide properties-correcting agent 201.2g.
The 9g coal ash fiber is dispersed in the 3000ml water, soaked 20 minutes, add the 0.35g polyacrylic acid amide modifier, stirred 15 minutes, and added the 18g wood pulp cellulose again, stirred 5 minutes, stop to stir, papermaking on the sheet forming machine then obtains containing the paper of coal ash fiber.
Claims (5)
1. the preparation of a polyacrylic acid amide modifier for fly ash fiber paper making and application method, it is characterized in that: at aqueous phase acroleic acid polymerization is become polyacrylic acid earlier, with N, N-dimethyl-1,3-propylene diamine join and carry out amidation in the polyacrylic acid aqueous solution again; The gained amidated products is warming up to 50～80 ℃, and the adding bromination of n-butane carries out quaternized, obtains polyacrylic acid amide modifier.Then, coal ash fiber is dispersed in the water, adds polyacrylic acid amide modifier, stirred 10～15 minutes, interpolation xylon slurry, after mixing, papermaking on the sheet forming machine obtains containing the paper of coal ash fiber.
2. the described N of claim 1, N-dimethyl-1, the add-on of 3-propylene diamine is: vinylformic acid and N, N-dimethyl-1, the molar ratio of 3-propylene diamine are 1: 1～3: 1.
3. the add-on of the described bromination of n-butane of claim 1 is: bromination of n-butane and acrylic acid molar ratio are 1: 1.
4. claim 1 is described adds polyacrylic acid amide modifier at the coal ash fiber aqueous phase, and its add-on is: in the oven dry weight polyacrylic acid amide modifier is 1～10% of coal ash fiber.
5. described coal ash fiber of claim 1 and xylon, in dry pulp weight coal ash fiber: wood pulp cellulose is 1: 2.
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| CN 201010202753 CN101870748B (en) | 2010-06-17 | 2010-06-17 | Preparation and application methods of polyacrylic acid amide modifier for fly ash fiber paper making |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102720057A (en) * | 2012-07-03 | 2012-10-10 | 河南省科学院化学研究所有限公司 | Fibre material containing quaternary ammonium groups and synthetic method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580391A (en) * | 2004-05-18 | 2005-02-16 | 华东理工大学 | Flyash fiber pulp and papermaking method using same as raw material |
| CN1843992A (en) * | 2006-04-03 | 2006-10-11 | 彭苏宁 | Wind cooling method for preparing fiber by fly ash and apparatus thereof |
| CN101250032A (en) * | 2008-03-24 | 2008-08-27 | 华东理工大学 | Technology for coal ash fibre surface treatment and use of asphalt reinforcing modification thereof |
-
2010
- 2010-06-17 CN CN 201010202753 patent/CN101870748B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580391A (en) * | 2004-05-18 | 2005-02-16 | 华东理工大学 | Flyash fiber pulp and papermaking method using same as raw material |
| CN1843992A (en) * | 2006-04-03 | 2006-10-11 | 彭苏宁 | Wind cooling method for preparing fiber by fly ash and apparatus thereof |
| CN101250032A (en) * | 2008-03-24 | 2008-08-27 | 华东理工大学 | Technology for coal ash fibre surface treatment and use of asphalt reinforcing modification thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102720057A (en) * | 2012-07-03 | 2012-10-10 | 河南省科学院化学研究所有限公司 | Fibre material containing quaternary ammonium groups and synthetic method thereof |
| CN102720057B (en) * | 2012-07-03 | 2014-04-30 | 河南省科学院化学研究所有限公司 | Fibre material containing quaternary ammonium groups and synthetic method thereof |
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| CN101870748B (en) | 2013-03-20 |
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