CN100510256C - Pulverous sizing agent synthesis process - Google Patents

Pulverous sizing agent synthesis process Download PDF

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CN100510256C
CN100510256C CNB2007100226756A CN200710022675A CN100510256C CN 100510256 C CN100510256 C CN 100510256C CN B2007100226756 A CNB2007100226756 A CN B2007100226756A CN 200710022675 A CN200710022675 A CN 200710022675A CN 100510256 C CN100510256 C CN 100510256C
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hours
glue
minutes
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CN101086147A (en
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邵百成
何方
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SHE COUNTY BAIYI FINE CHEMICAL FACTORY
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SHE COUNTY BAIYI FINE CHEMICAL FACTORY
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Abstract

The invention discloses a synthesis art of powder sizing agent, it includes glue reaction procedure, glue dispersing procedure and drying procedure; compared with prior technology, the invention replaces the rosin resin with oil resin, saves cost and it is helpful for the protection of forestry and ecological environment.

Description

A kind of synthesis technique of pulverous sizing agent
Technical field:
The invention belongs to this technical field of synthetic process of sizing agent, belong to this technical field of synthesis technique of paper grade (stock) pulverous sizing agent especially.
Background technology:
Sizing agent is mainly used in the paper technology, and paper pulp is carried out applying glue, improves the anti-water and the anti-permeability performance of paper, and the use amount of paper per ton is 5-10kg.Sizing agent is divided into two kinds of emulsion form and pulverous sizing agents, and the emulsion form sizing agent is difficult for storing, transportation, and use cost is also high, and therefore the pulverous sizing agent that is easy to transport becomes the trend of present sizing agent development.
" papermaking chemical product " 1996.3 introduced the easy molten AKD neutral sizing agent of a kind of powdery, and its technical scheme is for to wrap the AKD particulate with the examples of suitable agent, and it is bonding that it is not taken place each other, gets final product through spray drying again.
The production technology that a kind of powdery is strengthened sizing agent has been introduced in " Zhejiang papermaking " 1997.2, its technical scheme is with rosin and cis-butenedioic anhydride Di-A Fanying to take place earlier, generate 115 maleic rosins, adding alkali lye again disperses, carry out defoaming treatment with paraffin, form solid content and be 50% glue, enter again and carry out spray drying in the spray drying tower and get final product.
Above-mentioned two kinds of methods all are that existing sizing agent is carried out drying with spray drying, the production cost height.
Summary of the invention:
Technical problem to be solved by this invention provides the synthesis technique of the low pulverous sizing agent of a kind of cost.
The technical scheme of technical solution problem of the present invention is: a kind of synthesis technique of pulverous sizing agent comprises glue reaction process, glue dispersion step, drying process:
Described glue reaction process is: the maleic anhydride of Petropols and capacity is reacted under 190-200 ℃ condition be not less than 5 hours, add rosin, after treating the rosin fusing, add remaining maleic acid anhydride reactant and be not less than 4 hours, be warming up to 200-210 ℃, add the reaction of fumaric acid and paraffin again and be not less than 2 hours, add the carboxymethyl starch of gelatinization again, reaction is not less than 2 hours, is cooled to room temperature and gets final product;
Oil rosin: maleic anhydride; Fumaric acid: paraffin: the weight ratio of gelatinization carboxymethyl starch is=100:15-18:6-8:6-7:80-90;
Described glue dispersion step is: the sizing material and the dispersant that prepare in the glue reaction process are not less than 20 minutes 100-150 ℃ of reactions, deliver to the homogenizer homogeneous again and be not less than 30 minutes, the material that homogeneous is good is cooled to 90-95 ℃, add the polyacrylamide reaction and be not less than 30 minutes, be cooled to room temperature, filtration gets final product; The weight ratio of sizing material, dispersant, polyacrylamide is 1:0.3-0.8:0.01-0.05;
Described dispersant prepares by following method:
Modified starch is added an amount of water stir, be warming up to 40-45 ℃, add highly basic or strong base solution, after adding, be warming up to 70-80 ℃, add etherifying agent, be warming up to 85-90 ℃ again, reaction is not less than 1 hour, adds acetic acid, reacts down at 90-95 ℃ to be not less than 2 hours, add remaining water again, stirring is not less than 20 minutes, filters, and the weight ratio of modified starch, water, alkali, etherifying agent, acetic acid is 1:0.8-1.2:2-5:2-5:0.03-0.06;
Certainly, the present invention also can utilize existing spray drying operation to carry out drying.
Described drying process also can be: under 75-80 ℃ condition, stirring at low speed is not less than 80 minutes with scattered glue, and insulation is not less than 4 hours, be cooled to room temperature, material be crushed to be not more than 80H, be warming up to 80-90 ℃ again, insulation is not less than 6 hours, is cooled to the room temperature pulverizing and gets final product.
For the granularity that makes pulverous sizing agent is more even, in the glue dispersion step, can carry out above homogeneous twice.
In the glue reaction process, the molecular weight of Petropols is preferably 700-800, and Petropols are C 9, C 5It is a kind of or the mixture of two kinds of Petropols.
C 9, C 5When system was mixed, its weight ratio was: C 9System: C 5System=1:0.80-1.8.
Described C 9The through-stone oleoresin is polymerized by styrene, a-methyl styrene, methyl styrene, indenes etc.The softening point of this resin is 80~150 ℃, mean molecule quantity 1000~1500, and bromine valency 30, acid number is lower than 1.
Described C 5The through-stone oleoresin is polymerized by cyclopentadiene, isoprene, pentadiene, 2-methyl-1-butene alkene, 2-methyl-2-butene etc.The softening point of this resinoid is 70~100 ℃, and acid number is lower than 1, relative density 0.96.
In the dispersant preparation section, the model of described modified starch is preferably MS-01 starch, and the model of etherifying agent is 188 type etherifying agents.
The present invention is a main raw material with Petropols, rosin, carboxymethyl starch, carries out repeatedly carboxylatedly, adds dispersant special, carry out high-pressure homogeneous reaction, add polyacrylamide again, after disperseing reaction, produce aqueous sizing material, more aqueous sizing material drying is made finished product.
The present invention compared with prior art has the following advantages:
1, Petropols is substituted abietic resin, saved cost, also be beneficial to protection forestry ecological environment.
2, introduce hydrophilic carboxylic acid group in the molecular structure of Petropols, the Petropols after the modification and rosin acid have the certain structure similitude, after the blend again through and the cis-butenedioic anhydride heat polymerization, thereby successful make two kinds of materials crosslinked.
3, mixed material is repeatedly carboxylated, regulate the activated double bonds number that mixes crosslinked resin, and changed the distribution of carboxyl key.
4, utilized the emulsion dispersion property of modified starch, make this starch not only emulsification disperseed colloidal medium, more brought into play the premium properties of its top sizing.
The specific embodiment:
The present invention will be described in detail below in conjunction with embodiment:
Embodiment 1:
1, preparation gelatinization carboxymethyl starch.
In enamel reaction still, feed intake: 1000 kilograms in water, 100 kilograms of carboxymethyl starch, thrown the material after, stirred 30 minutes, after be warming up to more than 90 ℃, timing insulated and stirred 2 hours is cooled to 60 ℃ of blowings, the mistake 80 mesh sieves filter the gelatinization carboxymethyl starch.
2, preparation dispersant
With 400 kilograms in water, 200 kilograms of MS-01 starch stirred 15 minutes, when being warming up to 40 ℃, begin to drip weight concentration and be 30 NaOH solution, dropwised in 30 minutes, add 42 kilograms of alkali lye altogether, be warming up to 70 ℃, add 70 kilograms of 188 type etherifying agents, be warming up to 90 ℃ again,, add 8 kilograms in glacial acetic acid 85-90 ℃ of reactions 1 hour, reacted 2 hours down at 90-95 ℃, add 200 kilograms of entry, stir after 20 minutes, blowing, centrifugal filtration gets dispersant.
3, glue reaction process.
With mean molecule quantity is that 700-800 Petropols are with C 9300 kilograms, 36 kilograms of maleic anhydrides have been thrown material and have been warming up to 190 ℃, stir,, add 200 kilograms of rosin again 190-200 ℃ of following insulation reaction 5 hours, after stir melting, add 18 kilograms of maleic anhydrides, 190-200 ℃ of following insulation reaction 4 hours, add 10 kilograms of fumaric acid again, 10 kilograms in paraffin 200-210 ℃ of following insulation reaction 2 hours, adds 170 kilograms of carboxymethyl starch gelatinization sizing materials, stir after 30 minutes, generate blend glue stuff.
4, glue dispersion step:
Feeding intake in (1500r/min) emulsion tank at a high speed: with 300 kilograms of the blend glue stuffs in the glue reaction process, add the dispersant 120 kg, between 100-150 ℃, emulsion reaction 20 minutes is delivered to the high pressure homogenizer that pressure is 40MPa again, adds 5 kilograms of the polyacrylamide of molecular weight more than 300,000,90-95 ℃ of reactions 1 hour, sheared 15 minutes through the 1200r/min dispersion impeller, blowing, centrifugal filtration obtains the dispersion and emulsion sizing material.
5, drying process is existing spray drying operation.
Embodiment 2:
Removing drying process is:
Scattered sizing material is tiled in the stainless steel pallet, expect thick 15-20cm, move in 75-80 ℃ the drying room, dried by the fire 4-5 hours, again material is cooled off, pour into after the cooling in the baking pot, the baking pot temperature is 180-200 ℃, stirs 10 minutes under the condition of 15r/min, again material is crushed to 80-100 orders through pulverizer, material after the pulverizing reinstalls in the pallet, expects thick 30-40cm, moves on in 80-90 ℃ the drying room, dried by the fire 6-8 hours, shift out cooling, promptly make outside the powdery SBC sizing agent finished product, all the other are identical with embodiment 1.
Embodiment 3:
Removing at the used raw material of glue reaction is C 9, C 5Petropols mix in system, and its weight ratio is: C 9System: C 5Outside the system=1:1.5, all the other are identical with embodiment 2.
Solubility of the present invention detects according to the method for GB 13025.4.
Volatile matter of the present invention detects according to the method for GB 5528.
1% quality solution viscosity of the present invention detects according to the method for GB 10247.
The density of 1% concentration solution of the present invention detects according to the method for GB 4472.
The outward appearance of embodiment 1-3 is the faint yellow solid powder.
Table 1:
Solubility (%) Volatile matter (%) 1% quality solution viscosity (mp as) Density (the g/cm of 1% concentration solution 2)
Embodiment 1 99 15 5 1.0
Embodiment 2 99 18 5 1.0
Embodiment 3 99 18 5 1.0

Claims (4)

1, a kind of synthesis technique of pulverous sizing agent comprises glue reaction process, glue dispersion step, drying process:
Described glue reaction process is: the maleic anhydride of Petropols and capacity is reacted under 190-200 ℃ condition be not less than 5 hours, add rosin, after treating the rosin fusing, add remaining maleic acid anhydride reactant and be not less than 4 hours, be warming up to 200-210 ℃, add the reaction of fumaric acid and paraffin again and be not less than 2 hours, add the carboxymethyl starch of gelatinization again, reaction is not less than 2 hours, is cooled to room temperature and gets final product;
Petropols: maleic anhydride: fumaric acid: paraffin: the weight ratio of gelatinization carboxymethyl starch is=100:15-18:6-8:6-7:80-90;
Described glue dispersion step is: the sizing material and the dispersant that prepare in the glue reaction process are not less than 20 minutes 100-150 ℃ of reactions, deliver to the homogenizer homogeneous again and be not less than 30 minutes, the material that homogeneous is good is cooled to 90-95 ℃, add the polyacrylamide reaction and be not less than 30 minutes, be cooled to room temperature, filtration gets final product; The weight ratio of sizing material, dispersant, polyacrylamide is 1:0.3-0.8:0.01-0.05;
Described dispersant prepares by following method:
Modified starch is added an amount of water stir, be warming up to 40-45 ℃, add highly basic or strong base solution, after adding, be warming up to 70-80 ℃, add etherifying agent, be warming up to 85-90 ℃ again, reaction is not less than 1 hour, adds acetic acid, reacts down at 90-95 ℃ to be not less than 2 hours, add remaining water again, stirring is not less than 20 minutes, filters, and the weight ratio of modified starch, water, alkali, etherifying agent, acetic acid is 1:0.8-1.2:2-5:2-5:0.03-0.06.
2, the synthesis technique of a kind of pulverous sizing agent according to claim 1 is characterized in that:
Described drying process is: under 75-80 ℃ condition, stirring at low speed is not less than 80 minutes with scattered glue, and insulation is not less than 4 hours, be cooled to room temperature, material be crushed to be not more than 80 orders, be warming up to 80-90 ℃ again, insulation is not less than 6 hours, is cooled to the room temperature pulverizing and gets final product.
3, the synthesis technique of a kind of pulverous sizing agent according to claim 1 is characterized in that: in the glue reaction process, the molecular weight of Petropols is 700-800, and Petropols are C 9, C 5It is a kind of or the mixture of two kinds of Petropols.
4, the synthesis technique of a kind of pulverous sizing agent according to claim 3 is characterized in that: C 9, C 5When system was mixed, its weight ratio was: C 9System: C 5System=1:0.80-1.8.
CNB2007100226756A 2007-05-25 2007-05-25 Pulverous sizing agent synthesis process Expired - Fee Related CN100510256C (en)

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CN103233393A (en) * 2013-04-03 2013-08-07 安徽百翼生物科技有限公司 Preparation method for special sizing agent for polycarboxylic acid hardboard
CN103866620B (en) * 2014-02-25 2016-04-13 苏州恒康新材料有限公司 A kind of carboxymethyl starch sizing agent and preparation method thereof
CN104119700B (en) * 2014-07-08 2016-04-27 东北林业大学 The preparation method of starch under a kind of ultrasonic assistant/rosin inclusion compound base modified filler
CN106676967B (en) * 2016-12-11 2018-11-06 嘉兴尚云自动化设备有限公司 A kind of preparation method of environmental protection breathable stable type fruit cultivating bag paper Cypres
CN114892440A (en) * 2022-05-15 2022-08-12 成都奥睿尔科技创新服务有限公司 Special glue applying powder for packaging paper

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