Preparation method of modified AKD (Alkyl Ketene Dimer)

neutral sizing agent

CN 102337707 A
TM TT
The invention relates to a modified AKD (Alkyl Ketene Dimer) neutral sizing agent which is a milk
white liquid in appearance. The modified AKD neutral sizing agent comprises the following main
materials: AKD, starch, paraffin, high molecular dispersant and other assistant materials. The modified
AKD neutral sizing agent is mainly used for sizing paper pulp and improving the water resistance and
impermeability of paper in the paper-making production process, and the consumption for every ton of
paper is 10-20kg. Compared with like products, the quickly-cured modified AKD neutral sizing agent
has the following advantages: (1) effective ingredient particles of the product are finer and more
uniform and can be cured more tightly, the product has a longer quality guarantee period, and
convenience is provided for transportation and storage; (2) the product is applicable to neutral paper
pulp and can no longer result in the production of acidic paper-making sewage, thereby being
beneficial to environmental protection; (3) the use effect of the product can act quickly, and the curing
time is extremely short, thereby facilitating the effect monitoring and quality control in use, improving
the production efficiency and enhancing the yield of paper; and (4) the consumption of the product is
lower than that of other like products, thereby reducing the cost of production materials and improving
the economic benefits of customers.

LI XC NHN(8) c dch t Ting Trung

1. Modified AKD neutral sizing agent, characterized in that the preparation method is the plastic
materials and starch dispersing agent and an amount of dilution water, after mixing, heated to 80-90
C, followed by the addition of alkyl ketene mer, the resulting blend paraffin binding material, between
60-80 C were 1500r / minr high speed emulsification for 15 minutes, then passed through a high
pressure homogenizer 40MPa, pressure homogenized, homogenized compound After passing
through a plate heat exchanger, rapid cooling, adding a certain amount of dilution water and aluminum
sulfate solution, prepared as a finished product.
Modification according to claim 1, wherein the neutral sizing agent AKD, wherein: the weight ratio of
each component according to: alkyl ketene dimer: Paraffin: Dispersant: starch gum: aluminum sulfate
solution: dilution water = 90: 10: 100: 100: 200: 500
Modification according to claim 1, wherein the neutral sizing agent AKD, wherein: said alkyl ketene
dimer is an alkyl ketene dimer type 1840, the synthetic material, 18 carbon chain fatty acid containing
40% number.
According to claim 1, wherein the modified AKD neutral sizing agent, characterized in that: the 58 fully
refined paraffin wax.
AKD modified according to claim 1, wherein the neutral sizing agent, characterized in that: said
dispersant in various chemical and other chemical material monomer polymerization, is dissolved
oxidized tapioca starch gelling material , sodium hydroxide (99%) of a substitution reaction, and a
solution of 3-chloro-2-hydroxypropyl - trimethyl ammonium chloride (69%) of graft reaction; plus
glacial acetic acid, acrylamide solution ( 40%), N- methylol acrylamide solution polymerization, tert-

dodecyl mercaptan to control molecular weight, using ammonium persulfate as the initiator, and then
Gaja sodium methylene bis tea, in order to improve dispersibility.
AKD modified according to claim 1, wherein the neutral sizing agent, characterized in that: said
compound is a cationic starch as the main raw cassava starch polymerization, first dissolving the
compound to a cationic tapioca starch, was heated to 90 C-95 C under pasting, a "liquefaction"
effect with -type amylase, hydrolyzed starch molecules in a-1.4 glucosidic bond, generating a small
amount of short chain low molecular weight dextrins and sugars, then add acrylamide solution (40%),
was added dimethyl diallyl ammonium chloride is polymerized, using ammonium persulfate as the
initiator, and then glacial acetic acid to adjust the PH value, and then added to the chitosan
polymerization, in order to improve retention performance .
AKD modified according to claim 1, wherein the neutral sizing agent, characterized in that: the ironfree aluminum sulfate solution is aluminum sulfate (aluminum oxide content> 16.5%) in water solution,
its various the weight ratio of component: iron-free aluminum sulfate: water = 100: 150
AKD modified according to claim 1, wherein the neutral sizing agent, characterized in that: said water
is deionized water.

M T c dch t Ting Trung

Preparation of modified AKD neutral sizing agent
[0001] Technical Field
[0002] The present invention pertains to a process for the preparation of chemical raw materials, more
particular description relates to a method for preparing a modified AKD neutral papermaking sizing
agent.
BACKGROUND
[0003] similar products available on the market mainly ordinary AKD emulsion, dispersed rosin, ASA
emulsions and other products, at these types of products have shortcomings:
Example One: General AKD emulsion: (1) a long maturation period, the effect appeared slow; (
product particulates easy to gather large particles; C3) use, easy to slip on paper.
[0004] Example 2: Dispersed Rosin: (1) is not suitable for use neutral pulp; O) easily layered, short
shelf life; (3) the need to use in conjunction with other aluminum-based material will be effective, high
customer production costs.
[0005] Example Three: ASA emulsion: (1) short shelf life, storage inconvenient; former O) using the
required site emulsification, operational problems; (3) the application of refractory unstable results.
SUMMARY

[0006] The object of the present invention is to provide a modified process for preparing AKD neutral
sizing agent to alkyl ketene dimer, paraffin, aluminum sulfate as the main raw material, adding
special-made polymer dispersing agent, special homemade plastic materials such as starch additive
materials prepared high shear emulsification process, high pressure homogenization reaction, rapid
cooling, etc., to obtain the finished product.
[0007] To achieve the above object, the present invention adopts the following technical scheme:
Modified AKD neutral sizing agent, its preparation method and a dispersant amount of plastic
materials and starch dilution water, mixed heated to 80-90 C, and then adding an alkyl ketene dimer,
paraffin combine to generate The blend material, between 60-80 C at high speed (1500r / min)
emulsified reaction for 15 minutes, and then passed through a high pressure homogenizer 40MPa,
pressure homogenizer, homogenized plastic material through the plate heat exchanger After rapid
cooling, adding a certain amount of dilution water and aluminum sulfate solution, prepared as a
finished product.
[0008] the components of the present invention, wherein a weight ratio of: alkyl ketene dimer: Paraffin:
Dispersant: starch gum: aluminum sulfate solution: diluted water = 90: 10: 100: 100: 200: 500.
[0009] The present invention is the alkylketene dimer type is 1840 (synthesis of raw materials, the
number of 18 carbon chain fatty acid containing 40%.) Alkyl ketene dimer.
[0010] The invention described paraffin for 58 fully refined paraffin wax.
[0011] The dispersant of the present invention in various other chemical materials and chemical
monomers polymerized. Is dissolved into a compound oxidized tapioca starch, sodium hydroxide
(99%) in a substitution reaction, and a solution of 3-chloro-2-hydroxypropyl - trimethyl ammonium
chloride (69%) grafting reaction.Coupled with glacial acetic acid, acrylamide solution (40%), Nmethylol acrylamide solution polymerization, tert-dodecyl mercaptan to control molecular weight,
using ammonium persulfate as the initiator. Sodium methylene bis tea Gaja again, in order to improve
dispersibility.
[0012] starch gum according to the present invention is the cationic tapioca starch as the main raw
material polymerization.First dissolving the compound into a cationic tapioca starch, and heated to 90
C-95 C under pasting, a "liquefaction" effect with -type amylase, hydrolyzed starch molecules in
a-1.4 glucosidic bond, generating short chain dextrin and small amounts of low molecular weight
sugars, and then added a solution of acrylamide (40%), was added dimethyl diallyl ammonium
chloride is polymerized, using ammonium persulfate as the initiator, and then glacial acetic acid to
adjust the pH value, added shell glycans further polymerized to improve retention performance.
[0013] The aluminum sulfate solution of the present invention is iron-free aluminum sulfate (aluminum
oxide content> 16.5%) solution in water. The weight ratio of each component are: iron-free aluminum
sulfate: water = 100: 150.

[0014] Water according to the present invention is deionized water.

[0015] Compared with existing technologies, the present invention successfully introduced AKD wax
neutral sizing agent of the production and improve the water resistance AKD neutral sizing agent and
the like, the present invention is the successful synthesis of a dispersing agent, This is a polymer
dispersant, better emulsification stability and permeability and other properties, so that the joint
material and the alkyl ketene dimer wax more soluble, dispersible. The present invention successfully
synthesized starch gum, which is a polymer retention agent, improved stability and sizing
efficiency. The combined materials and AKD wax, synthetic dispersants, starch compounds, the high
shear emulsification and high pressure homogenization reaction, raw style soluble colloids, adding
aluminum sulfate solution and diluted with water to prepare modified AKD neutral sizing agent. The
product quality and product results appear quickly, a small amount of high efficiency, low cost.
DETAILED DESCRIPTION
[0016] 1. Preparation of Dispersant
In enamel autoclave feed:
1.1, raw material formulation: 1000.0 kg Total Production
1. 1.1, oxidized cassava starch: 108 0 kg; oxidized cassava starch by the Guangxi Mingyang
Biochemical Co., Ltd. produced MS-Ol-type starch.
[0017] 1. 1.2, sodium hydroxide (99%): 7.5 kg;
1. 1. 3,69% 3_ chloro-2-hydroxypropyl - trimethyl ammonium chloride: 38 0 1 1.4 kg, tert-dodecyl
mercaptan: 2 0 kg;.
. 1. 1. 5, N- methylol acrylamide solution: 2 5 kg of N- methylol acrylamide is dissolved, add water
40.0 kg, mixing uniformly;
1. 1. 6,40% acrylamide solution: 178 0 kg;
1.1.7, TX-10 emulsifier solution: TX-10 emulsifier 5 kg 25 kg of water to dissolve and mix well;
1. 1.8, glacial acetic acid: 14.0 kg;
1. 1.9, methylene bis tea Sodium: 13 0 kg;
1. 1.10, ammonium persulfate solution: 3.0 kg water 80 kg of ammonium persulfate were dissolved
and mixed uniformly.
[0018] 1. 1.11, water: 484.0 kg

1.2, in 1000 l autoclave reaction of the production process

1. 2.1, to 238.0 kg of water added to the kettle, oxidized tapioca starch was added with stirring and
heated to 40 C, heated for 30 minutes;
1. 2.2, was added sodium hydroxide (99%), was heated to 60-65 V, constant temperature for 30
minutes, began dropping 69% 3-chloro-2-hydroxypropyl - trimethyl ammonium chloride, After heating
to a constant temperature of 70 C _75 C for 3 hours;
1. 2.3, adding 86.0 kg of water, glacial acetic acid, 40% acrylamide solution, coupled with tert-dodecyl
mercaptan, nitrogen 30 minutes; 1.2 4, then began dropping emulsifier (TX- 10) was added dropwise
a solution of N- methylol acrylamide, 30 minutes After the dropwise addition, while a solution of
ammonium persulfate solution, five-sixths of 40 minutes was added dropwise a solution of the
complete, to stay more than one sixth, the material at 850C -88 C and incubated for 1 hour;
1. 2.5, 10 minutes and then dropped completely leaving the remaining ammonium persulfate solution,
insulation materials for 2 hours under 78V _82 C; 160.0 kg of water, plus dispersant N, heated to 90
C, heat for 30 minutes, cooled to 50 C to discharge, based products dedicated dispersant.
[0019] 1000 kg of water, 100 kg of carboxymethyl starch, feeding After stirring for 30 minutes, after
heating to 90 C above, the timing insulation stirred for 2 hours, cooled to 60 C discharge, over 80
mesh sieve was carboxymethyl starch pasting gum.
[0020] 2. Preparation of starch gel material in the reactor feed enamel:
2.1, raw material formulation: 1000.0 kg Total Production
2. 1.1, cationic tapioca: 125 0 kg; cationic starch from cassava in Guangxi Mingyang Biological
Chemical Co., CS-08 type of starch.
. [0021] 2. 1. 2, -type amylase: 0 15 kg; 2. 1. 3,40% acrylamide solution: 35.0 kg;
2. 1.4, diallyl dimethyl ammonium chloride: 50 0 kg; 2. 1.5, chitosan: 1.1 kg; 2. 1.6, glacial acetic acid:
14.0 kg;
2. 1.7, ammonium persulfate solution: 2.75 kg 45.0 kg of water to dissolve and mix well.
[0022] 2. 1.8, Water: 727.0 kg.
[0023] 2.2, in a 1000 liters reactor in the reaction of the production process
2.2.1, was added 400.0 kg of water, addition of a cationic starch, was added -type amylase, and
heated to a constant temperature at 900C -95 C for 1 hour;

2. 2.2, was added 80.0 kg of water, 40% acrylamide solution was added, with stirring was added
dimethyl diallyl ammonium chloride, nitrogen, a solution of ammonium persulfate solution for 2 hours,
and heated to 80- 82 C, the constant temperature for 3 hours;
2. 2.3, nitrogen gas was stopped, was added M7. 0 kg of water, glacial acetic acid, was added
chitosan, warmed to 90 C, for 2 hours, cooled to 50 C to discharge, based products dedicated
starch compound.
[0024] 3, aluminum sulfate solution prepared
In enamel kettle feed: The 400.0 kg iron-free aluminum sulfate was added 600.0 kg of water, stirred
for 1 hour or until most of the solids had dissolved, another 100 mesh screen filter.
[0025] 4. Preparation of the finished product
4.1, in a stainless steel autoclave feed: 90 0 kg AKD wax and 10.0 kg, melt to 65-70 C, stir;.
4.2, in 1500r / min high speed emulsification tank feeding:... 100 0 kg homemade special dispersants,
100 0 kg special starch gum made, 300 0 kg of water, stirred, and heated to 85-90 C ;
4.3, the alkyl ketene dimer and melted paraffin mixture, was added 1500r / min speed emulsification
tank material, the shear via a high speed disperser for 15 minutes and discharge, through an 80 mesh
screen filter to give dispersed emulsion rubber;
4.4, the dispersion was emulsified plastic material fed 40MPa high pressure homogenizer,
homogenized under reduced pressure, after gum after homogenization through the plate heat
exchanger, rapid cooling to 25-30 C, was added 200.0 kg dilution water and 200.0 kg of aluminum
sulfate solution, stir, filtered through a 100 mesh screen, which was prepared for the finished product.