CN108752517A - A kind of formula and preparation method thereof of noctilucence bullet pearl - Google Patents
A kind of formula and preparation method thereof of noctilucence bullet pearl Download PDFInfo
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- CN108752517A CN108752517A CN201810555439.9A CN201810555439A CN108752517A CN 108752517 A CN108752517 A CN 108752517A CN 201810555439 A CN201810555439 A CN 201810555439A CN 108752517 A CN108752517 A CN 108752517A
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- noctilucence
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- bullet pearl
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The present invention relates to the preparation of water-absorbing resin and production technical fields, are concretely a kind of formulas and preparation method thereof of noctilucence bullet pearl, include the component of following weight content：20% ~ 40% monomer, 10% ~ 20% sodium hydroxide, 0.1% ~ 1% crosslinking agent, 0.1% ~ 0.5% catalyst, 0.2% ~ 5% dispersant, 1% ~ 5% thickener, 1% ~ 3% anti-settling agent, 2% ~ 8% luminescent powder；Preparation method is as follows：First, in accordance with requiring to weigh each component；Sodium hydroxide, water are mixed, monomer mixing, adjusts pH value, crosslinking agent, anti-settling agent is then added, obtains meta-acid mixture A1；Luminescent powder is added and is uniformly mixed with dispersant again, thickener is added afterwards, obtains meta-acid mixture A2；Catalyst is added later, it is made to form reaction system after mixing, is transferred in former, forms spherical drop, polymerisation is carried out into reaction kettle, after over cleaning, drying, obtains noctilucence bullet pearl.The shortcomings that disperseing uneven and poor toughness the present invention overcomes luminescent powder existing for noctilucence bullet pearl.
Description
Technical field
The present invention relates to the preparation of water-absorbing resin and production technical fields, are concretely a kind of formulas of noctilucence bullet pearl
And preparation method thereof.
Background technology
It is well known that the ingredient of toy gun bullet is water-absorbing resin, and it is a kind of functional high molecule material, it can be with water absorption and swelling
And preserve the macromolecule resin of moisture.Existing toy bullet pearl is only can be in the condition of daylight or other general light sources
Under be shot at, the function of noctilucence is not had under dark condition, inconvenience is brought to user.With science and technology
Development, raising of the people to spiritual quality requirements, modern night CS（True man's CS confrontation）More and more abundant colorful, traditional is commercially available
Common bullet pearl cannot meet the needs of modern night CS.
Invention content
The present invention breaches the problem of the prior art, and devise a kind of can send out colour bright under night dark condition
The formula and preparation method thereof of noctilucence bullet pearl.
In order to achieve the above object, the present invention devises a kind of formula and preparation method thereof of noctilucence bullet pearl, feature
It is：Include the component of following weight content：20% ~ 40% monomer, 10% ~ 20% sodium hydroxide, 0.1% ~ 1% crosslinking agent,
0.1% ~ 0.5% catalyst, 0.2% ~ 5% dispersant, 1% ~ 5% thickener, 1% ~ 3% anti-settling agent, 2% ~ 8% luminescent powder,
Surplus is water, and the weight percent content summation of above each component is 100%；
Preparation method is as follows：
Step 1：Each component is weighed as requested；
Step 2：After mixing by the sodium hydroxide weighed and water, monomer is added, adjusts pH value, make pH value range 6.0 ~
7.0, crosslinking agent, anti-settling agent is then added, obtains meta-acid mixture A1；
Step 3：Luminescent powder is uniform with dispersant, it is added in slant acidity mixture A1, is stirring evenly and then adding into thickening
Agent obtains meta-acid mixture A2；
Step 4：Catalyst is added in meta-acid mixture A2, so that it is formed reaction system after mixing, is transferred to former
In, spherical drop is formed, polymerisation is carried out into reaction kettle, controlling reaction temperature is 70 DEG C ~ 100 DEG C, reaction 5min ~
20min obtains noctilucence bullet pearl after over cleaning, drying；
In step 4, to keep the noctilucence bullet pearl produced uniform in size, liquid level in former need to be controlled and be fixed on 3-
20cm highly determines that height is different according to the particle size of noctilucence bullet pearl, and obtained grain size is different；Simultaneously because reaction
For exothermic reaction, therefore install refrigerating plant additional outside former, guarantee system temperature is stablized, to ensure the stability of product.
The monomer is one or more in acrylic acid, acrylic acid derivative or acrylic acid and acrylic acid derivative.
The crosslinking agent is ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, allyl methyl propylene
Acid esters, 1,1,1- trimethylolpropane acrylates, triallylamine, N, N- methylene-bisacrylamides, four allyloxy second
One or more of alkane.
The catalyst is selected from azodiisobutyronitrile, cerium salt, persulfate, persulfate-NaHSO3 systems, peroxidating
One or more of hydrogen-ascorbic acid system.
The dispersant is selected from sorbester p18, Tween 80, polysorbate85, OP-10, one kind or several in quaternary ammonium salt dispersant
Kind.
The thickener is selected from one or both of CMC or Sodium Polyacrylate.
The luminescent powder is one or more of zinc sulphide, calcium sulfide, terres rares luminescent powder.
The anti-settling agent is organobentonite, castor oil derivative, aerosil, polyolefin-wax, titanate esters coupling
One or more of agent and polyamide wax.
The former includes mainly barrel, SAPMAC method pipe, material mouth, if bottom is equipped with siccative mouth, the side of barrel in barrel
Face, which surrounds, is equipped with SAPMAC method pipe, the S shapes that the material mouth inner wall is in.
Compared with prior art, the present invention providing a kind of bullet pearl with luminous effect, while overcoming noctilucence
Luminescent powder existing for hoodle disperses the shortcomings that uneven and poor toughness, to facilitate user can be effective in modern night CS confrontation
Really stator launches outgoing direction or hides the attack of bullet, improves effect of playing.
Figure of description
Fig. 1 is the sectional view of former in the present invention.
Specific implementation mode
The present invention is described further in conjunction with attached drawing.
The present invention devises a kind of formula and preparation method thereof of noctilucence bullet pearl, it is characterised in that：Including following weight
The component of content：20% ~ 40% monomer, 10% ~ 20% sodium hydroxide, 0.1% ~ 1% crosslinking agent, 0.1% ~ 0.5% catalyst,
0.2% ~ 5% dispersant, 1% ~ 5% thickener, 1% ~ 3% anti-settling agent, 2% ~ 8% luminescent powder, surplus are water, above each group
The weight percent content summation divided is 100%；
Preparation method is as follows：
Step 1：Each component is weighed as requested；
Step 2：After mixing by the sodium hydroxide weighed and water, monomer is added, adjusts pH value, make pH value range 6.0 ~
7.0, crosslinking agent, anti-settling agent is then added, obtains meta-acid mixture A1；
Step 3：Luminescent powder is uniform with dispersant, it is added in slant acidity mixture A1, is stirring evenly and then adding into thickening
Agent obtains meta-acid mixture A2；
Step 4：Catalyst is added in meta-acid mixture A2, so that it is formed reaction system after mixing, is transferred to former
In, spherical drop being formed, then the droplet transfer to reaction kettle is subjected to polymerisation, controlling reaction temperature is 70 DEG C ~ 100 DEG C,
5min ~ 20min is reacted, after over cleaning, drying, obtains noctilucence bullet pearl；
In step 4, to keep the noctilucence bullet pearl produced uniform in size, liquid level in former need to be controlled and be fixed on 3-
20cm highly determines that height is different according to the particle size of noctilucence bullet pearl, and obtained grain size is different；Simultaneously because reaction
For exothermic reaction, therefore install refrigerating plant additional outside former, guarantee system temperature is stablized, to ensure the stability of product.
Monomer is acrylic acid, acrylic acid derivative or one kind or more in acrylic acid and acrylic acid derivative in the present invention
Kind.
Crosslinking agent is ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, allyl methyl in the present invention
Acrylate, 1,1,1- trimethylolpropane acrylates, triallylamine, N, N- methylene-bisacrylamides, four allyl oxygen
One or more of base ethane so that react more stable in reaction process, produce product yield height, good weatherability is protected
The matter phase is long.
Catalyst is selected from azodiisobutyronitrile, cerium salt, persulfate, persulfate-NaHSO3 systems, peroxide in the present invention
Change one or more of hydrogen-ascorbic acid system.The above catalyst is selected, is since polymerization-filling of the present invention itself belongs to
Free radical polymerization, the above catalyst is free radical type initiator, and dissolubility is good in system, can be evenly distributed on body
In system, to ensure that the uniformity of product, performance are consistent.
Dispersant is selected from sorbester p18, Tween 80, polysorbate85, OP-10 in the present invention, one kind in quaternary ammonium salt dispersant or
It is several, in dispersion process, since dispersed effect of the luminescent powder in water-based system is poor, easily reunite the phenomenon that, cause its
Product luminous effect is influenced in production, the present invention installs one additional on polyplant and is dispersed with stirring device, forms polymerization dispersion dress
It sets, what is made is carried out at the same time stirring in fill process so that the feed liquid moment is in a finely dispersed state, while controlling material
The page height of liquid is within 3-20cm so that polymerization process can be rapidly completed, this whole technique can promote to produce uniformly
Spend higher product.
Thickener is selected from one or both of CMC, Sodium Polyacrylate in the present invention, and selected thickener is in system
Good dispersion, may be homogenously dispersed in system, and thickening effect is good, effect can reach using a small amount of, to ensure
It can be further reduced the cost under the premise of product quality.
Luminescent powder is one or more of zinc sulphide, calcium sulfide, terres rares luminescent powder, common luminescent powder in the present invention
The radioactive luminescent powder of tool mostly, luminous effect is preferable, but its to environment, to human health, night of the invention
Light powder be it is "dead", it is beneficial to environment, health, at the same by adjust luminescent powder addition can adjust bullet pearl
Luminous effect.
Anti-settling agent is organobentonite, castor oil derivative, aerosil, polyolefin-wax, titanate esters in the present invention
One or more of coupling agent and polyamide wax are easy sedimentation in water-based system, cause since noctilucence powder density is larger
The content for being easy to be formed upper layer feed liquid luminescent powder in entire building-up process tails off, and one that the noctilucence powder content change of lower part is more is existing
As disperseing unevenness so as to cause the noctilucence of product, influencing the whole luminous effect of product.Anti-settling agent in the present invention, can be to prevent
Only luminescent powder settles in process of production so that luminescent powder can be uniformly dispersed in entire feed liquid, ensure the equal of product
Even property, to ensure the luminous effect of product.
Former includes mainly barrel 1, SAPMAC method pipe 2, material mouth 3 in the present invention, if bottom is equipped with siccative mouth 3 in barrel 1,
The side of barrel 1, which surrounds, is equipped with SAPMAC method pipe 2, the S shapes that 3 inner wall of material mouth is in, after may make feed liquid to enter drip nozzle by barrel,
It can get one to buffer and obtain uniform droplet size and uniform initial velocity under conditions of certain power, to ensure to produce
The uniformity of product size.
Embodiment 1：
The noctilucence bullet pearl of a diameter of 7mm ~ 8mm is prepared, formula is as follows：
| Monomer | 30% |
| Sodium hydroxide | 15% |
| Diethylene glycol dimethacrylate | 0.5% |
| Azodiisobutyronitrile | 0.3% |
| OP-10 | 0.2% |
| CMC | 2% |
| Aerosil | 1.5% |
| Terres rares luminescent powder | 6% |
| Deionized water | 44.5% |
Wherein monomer is made of acrylic acid, acrylic acid derivative, and its ratio be acrylic acid：Acrylic acid derivative=3:1.
Each component first is weighed according to aforementioned proportion, after mixing by the sodium hydroxide weighed and water later, is added third
Olefin(e) acid, acrylic acid derivative adjust pH value, make pH value range 6.7 or so, be then added diethylene glycol dimethacrylate,
Anti-settling agent aerosil obtains meta-acid mixture A1；
Terres rares luminescent powder is uniformly mixed with OP-10, is added in slant acidity mixture A1, is stirring evenly and then adding into CMC, obtains
Meta-acid mixture A2；Azodiisobutyronitrile is added in meta-acid mixture A2, it is made to form reaction system after mixing, shifts
Into former, the material mouth of former is changed to the material mouth that interior diameter is 7mm ~ 8mm, is added dropwise, controlling reaction temperature is
85 DEG C, reaction 15min obtains noctilucence bullet pearl through over cleaning, drying process.
Claims (9)
1. a kind of formula and preparation method thereof of noctilucence bullet pearl, it is characterised in that：Include the component of following weight content：20%~
40% monomer, 10% ~ 20% sodium hydroxide, 0.1% ~ 1% crosslinking agent, 0.1% ~ 0.5% catalyst, 0.2% ~ 5% dispersion
Agent, 1% ~ 5% thickener, 1% ~ 3% anti-settling agent, 2% ~ 8% luminescent powder, surplus is water, the weight percent of above each component
It is 100% than content summation；
Preparation method is as follows：
Step 1：Each component is weighed as requested；
Step 2：After mixing by the sodium hydroxide weighed and water, monomer is added, adjusts pH value, make pH value range 6.0 ~
7.0, crosslinking agent, anti-settling agent is then added, obtains meta-acid mixture A1；
Step 3：Luminescent powder is uniform with dispersant, it is added in slant acidity mixture A1, is stirring evenly and then adding into thickening
Agent obtains meta-acid mixture A2；
Step 4：Catalyst is added in meta-acid mixture A2, so that it is formed reaction system after mixing, is transferred to former
In, spherical drop is formed, polymerisation is carried out into reaction kettle, controlling reaction temperature is 70 DEG C ~ 100 DEG C, reaction 5min ~
20min obtains noctilucence bullet pearl after over cleaning, drying；
In step 4, to keep the noctilucence bullet pearl produced uniform in size, liquid level in former need to be controlled and be fixed on 3-
20cm。
2. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The monomer
It is one or more in acrylic acid, acrylic acid derivative or acrylic acid and acrylic acid derivative.
3. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The crosslinking
Agent is ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, allkyl methacrylate, tri- hydroxyl first of 1,1,1-
Base propane-propylene acid esters, triallylamine, N, one or more of N- methylene-bisacrylamides, tetraallyloxyethane.
4. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The catalysis
Agent is in azodiisobutyronitrile, cerium salt, persulfate, persulfate-NaHSO3 systems, hydrogen peroxide-ascorbic acid system
One or more.
5. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The dispersion
Agent is selected from sorbester p18, Tween 80, polysorbate85, OP-10, one or more of quaternary ammonium salt dispersant.
6. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The thickening
Agent is selected from one or both of CMC, Sodium Polyacrylate.
7. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The noctilucence
Powder is one or more of zinc sulphide, calcium sulfide, terres rares luminescent powder.
8. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：It is described anti-settling
Agent is in organobentonite, castor oil derivative, aerosil, polyolefin-wax, titanate coupling agent and polyamide wax
It is one or more of.
9. a kind of formula and preparation method thereof of noctilucence bullet pearl according to claim 1, it is characterised in that：The molding
Device includes mainly barrel（1）, SAPMAC method pipe（2）, material mouth（3）, barrel（1）If interior bottom is equipped with siccative mouth（3）, barrel（1）'s
Side, which surrounds, is equipped with SAPMAC method pipe（2）, the material mouth（3）The S shapes that inner wall is in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810555439.9A CN108752517A (en) | 2018-06-01 | 2018-06-01 | A kind of formula and preparation method thereof of noctilucence bullet pearl |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810555439.9A CN108752517A (en) | 2018-06-01 | 2018-06-01 | A kind of formula and preparation method thereof of noctilucence bullet pearl |
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| CN108752517A true CN108752517A (en) | 2018-11-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116751330A (en) * | 2023-07-25 | 2023-09-15 | 浙江三赢新材料有限公司 | High-stability noctilucent spherical water-absorbent resin and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927895A (en) * | 2005-09-09 | 2007-03-14 | 中国科学院理化技术研究所 | Nano-micron water-soluble microgel oil displacement material and preparation method thereof |
| CN107325220A (en) * | 2016-04-29 | 2017-11-07 | 上海创始实业（集团）有限公司 | A kind of heat discoloration water-absorbent resin composition and preparation method thereof |
-
2018
- 2018-06-01 CN CN201810555439.9A patent/CN108752517A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927895A (en) * | 2005-09-09 | 2007-03-14 | 中国科学院理化技术研究所 | Nano-micron water-soluble microgel oil displacement material and preparation method thereof |
| CN107325220A (en) * | 2016-04-29 | 2017-11-07 | 上海创始实业（集团）有限公司 | A kind of heat discoloration water-absorbent resin composition and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116751330A (en) * | 2023-07-25 | 2023-09-15 | 浙江三赢新材料有限公司 | High-stability noctilucent spherical water-absorbent resin and preparation method thereof |
| CN116751330B (en) * | 2023-07-25 | 2024-07-19 | 浙江三赢新材料有限公司 | High-stability noctilucent spherical water-absorbent resin and preparation method thereof |
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Effective date of registration: 20200110 Address after: 314107 No. 129 Ting Yao East Road, dry kiln industrial town, Jiashan County, Jiaxing, Zhejiang Applicant after: ZHEJIANG TRIPLE WIN NEW MATERIAL Co.,Ltd. Applicant after: Shanghai Chuangshi industry (Group) Co.,Ltd. Address before: 314107 No. 129 Ting Yao East Road, dry kiln industrial town, Jiashan County, Jiaxing, Zhejiang Applicant before: ZHEJIANG TRIPLE WIN NEW MATERIAL Co.,Ltd. |
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