CN109180961A - A kind of P (AM-co-St)@Bi of laser response2O3The preparation method and application of composite hydrogel - Google Patents
A kind of P (AM-co-St)@Bi of laser response2O3The preparation method and application of composite hydrogel Download PDFInfo
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Abstract
The invention belongs to macromolecule hydrogel and laser labelling field of material preparation, in particular to a kind of P (AM-co-St)@Bi of laser response2O3The preparation method and application of composite hydrogel.Hydrogel is a kind of with three-dimensional net structure and the good high molecular material of hydrophily.The invention firstly uses 3- (methacryloxypropyl) propyl trimethoxy silicanes (TMSPMA) to Bi2O3Powder is surface modified and introduces double bond, and with acrylamide (AAm) for principal monomer, and adds the styrene (St) with double bond and be modified, and prepares P (AM-co-St) Bi2O3Composite hydrogel.Laser response test is carried out to the hydrogel prepared.P (AM-co-St) the@Bi of this kind of specific laser response2O3Composite hydrogel is significant to the development in the laser labellings fields such as permanent marks, product false proof, the tracking of important spare part.
Description
Technical field
The invention belongs to macromolecule hydrogel and laser labelling field of material preparation, in particular to a kind of P of laser response
(AM-co-St)@Bi2O3The preparation method and application of composite hydrogel.
Background technique
Hydrogel is a kind of with three-dimensional net structure and the good high molecular material of hydrophily.In recent years, polypropylene
Amide hydrogel has important application because of its excellent water absorbing properties and tissue equivalent's property in many fields.Such as: it can be used to
Remove industrial wastewater in heavy metal ion, simulation building equivalent biological body tissue, and in daily life it is various extensively
Using etc..The further functionalization of polyacrylamide hydrogel, can improve its performance and expand its application range.
Hydrogel is in the research in laser labelling field and few, and bismuth oxide (Bi2O3) it is a kind of nothing that laser responds
Machine particle, is added in the preparation of hydrogel, can synthesize the hydrogel of laser response.Bismuth oxide (Bi2O3) be
A kind of powder of yellow.It has high refractive index and dielectric constant, optical nonlinearity and super fast response and significant photoelectricity
The property led and luminescence generated by light.These unique characteristics make Bi2O3Be suitable for multiple applications, for example, heterogeneous catalysis, sensor,
Electronics, optical coating, laser and glass manufacture.While studying hydrogel laser response effect, also to improve hydrogel
Comprehensive performance.Styrene (St) is a kind of common polymer modification material, and the chemical stability of material can be improved.
Documents patent CN102617837B discloses one kind can laser labelling PET quick crystallization polyester chip and its preparation
Method, PET polyester, laser mark auxiliary agent and crystallization nucleating agent are contained in the raw material of this method, and laser mark auxiliary agent is selected from dioxy
Change at least one of titanium, Sn/Sb mixed oxide or Sn/Ln mixed oxide, but process is tedious is not suitable for for its preparation process
Large-scale promotion production.Documents patent CN101243137B disclose a kind of intrinsic formability of holding polyamide,
The features such as mechanical properties, thermal stability, heat resistance, electrical characteristic and anti-flammability and the excellent polyamide resin of laser marking
Oil/fat composition, and laser labelling resin molded body obtained from being shaped, but the cost of this method it is not easy to control and
It is unfavorable for environmental protection.Therefore, it is necessary to develop a kind of laser responsive materials easy to operate, at low cost and environmentally friendly.Laser response type P
(AM-co-St)@Bi2O3Composite hydrogel is just having the feature that laser effect is ideal, at low cost and easy to operate and environmentally friendly, to forever
The development in the laser labellings fields such as long label, product false proof, the tracking of important spare part is significant.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods simply, laser response effect is ideal and comprehensive performance is good
P(AM-co-St)@Bi2O3The preparation method of composite hydrogel, to solve the problems mentioned in the above background technology.
The invention firstly uses 3- (methacryloxypropyl) propyl trimethoxy silicanes (TMSPMA) to Bi2O3Powder carries out
Surface modification simultaneously introduces double bond, and with acrylamide (AAm) for principal monomer, and adds the styrene (St) with double bond and carry out
It is modified, prepare P (AM-co-St)@Bi2O3Composite hydrogel.Wherein AAm is a kind of molecule of environmental response type, Bi2O3It is a kind of
The inorganic particle of laser response, St is a kind of common polymer modification material, and the chemical stability of material can be improved.
The present invention provides a kind of P (AM-co-St) the@Bi of photoresponse2O3Composite hydrogel preparation method, concrete technology is such as
Under:
Step (1): 40mL solvent is measured in 250mL beaker, bismuth oxide (Bi is added2O3), it stirs evenly, then plus
Enter 3- (methacryloxypropyl) propyl trimethoxy silicane (TMSPMA), and oil bath temperature is increased to 70 DEG C, reacts 2h, reaction
After collect product, place the product in 60 DEG C of vacuum drying oven to be dried, ground after drying, is obtained end and being changed with double bond
Property Bi2O3Particle.
Step (2): acrylamide (AAm) be principal monomer, be dissolved in solvent, be added with double bond styrene (St) into
Row is modified, and then adds the modification Bi that step (1) end has double bond again2O3Particle, and promotor, crosslinking agent and initiation is added
Agent prepares P (AM-co-St)@Bi by free radical polymerization2O3Composite hydrogel later mentions the composite hydrogel of preparation
It is pure, primary purification solution is changed every 8h, purification is for 24 hours.Acrylamide (AAm) the monomer structure formula is as follows:
The structural formula of the styrene (St) is as follows:
The structural formula of 3- (methacryloxypropyl) propyl trimethoxy silicane (TMSPMA) is as follows:
P (AM-co-St) the@Bi of the laser response2O3The preparation method of composite hydrogel, it is characterised in that: step
(1) TMSPMA and Bi in2O3Mass ratio be 1:5.
P (AM-co-St) the@Bi of the laser response2O3The preparation method of composite hydrogel, it is characterised in that: described
In step (2), N, N, N ', N '-tetramethylethylenediamine (TMEDA) is promotor；N, N '-methylene-bisacrylamide (MBA) is
Crosslinking agent；Potassium peroxydisulfate (K2S2O8) it is initiator, wherein the AAm, St being added, modified Bi2O3、TMEDA、MBA、K2S2O8Matter
Amount is than being 50:1~3:0~3:1~2:1~2:1~3, and polymeric reaction temperature is 25 DEG C, and polymerization reaction time is 6~8h.
In the step (1), solvent is deionized water；In step (2), solvent be n,N-Dimethylformamide (DMF) or
Deionized water is solvent, and the solution of purification is deionized water.
In the present invention, using semiconductor laser marking, to being not added with modified Bi2O3P (AM-co-St) hydrogel, P
(AM-co-St)@Bi2O3Composite hydrogel carries out laser response test respectively, and observes the best item of its laser response performance
Part.When laser current intensities are 16A, effect is ideal.
In the present invention, pass through the modified Bi of addition TMSPMA2O3Compound particle and St, hydrogel inside become porous regular knot
Modified Bi is added so that the compression performance of hydrogel is improved in structure2O3The composite hydrogel compression performance of particle is to be not added with
Modified Bi2O32~3 times of P (AM-co-St) hydrogel.Meanwhile P (AM-co-St) hydrogel and P (AM-co-St)@
Bi2O3The contact angle of composite hydrogel and water all has good hydrophily between 30 °~40 °.
The beneficial effects of the present invention are:
The present invention is by the above method, under conditions of without complicated preparation step, has synthesized the P with laser response
(AM-co-St)@Bi2O3Composite hydrogel.Compared to being not added with modified Bi2O3P (AM-co-St) hydrogel, be added be modified
Bi2O3Composite hydrogel laser labelling effect obviously improved.By adding modified Bi2O3Compound particle and St, hydrogel
Inside becomes porous ordered structure, so that the compression performance of hydrogel is improved, PS@Bi is added2O3The composite hydrogel of particle
Compression performance is to be not added with modified Bi2O32~3 times of P (AM-co-St) hydrogel.Meanwhile P (AM-co-St) hydrogel, P
(AM-co-St)@Bi2O3The contact angle of composite hydrogel and water all has good hydrophily between 30 °~40 °.
The present invention Bi modified using addition TMSPMA in hydrogel2O3Compound particle, so that Bi2O3Particle end has
Double bond, then reacted with the St with double bond and AAm, by free radical polymerization, double bond is opened, so that modified Bi2O3Grain
Son, St and AAm can link together, and form complicated network structure, prepare laser effect ideal and comprehensive performance is good
Composite hydrogel.Simultaneously in actual use, it is a kind of effective ways for being directly suitable for laser labelling, there is operation letter
Advantage single, at low cost and high-efficient, to laser labellings fields such as permanent marks, product false proof, the tracking of important spare part
Development it is significant.
Detailed description of the invention
Fig. 1 is P (AM-co-St) the@Bi of embodiment 1-4 preparation2O3Composite hydrogel picture (is from left to right modified
Bi2O3Mass content is successively 0,1%, 2% and 3%).
Fig. 2 is P (AM-co-St) the@Bi of embodiment 1-4 preparation2O3Picture after composite hydrogel laser labelling is (from a left side
To right modified Bi2O3Mass content is successively 0,1%, 2% and 3%).
Fig. 3 is embodiment 1-4 using different modified Bi2O3P (AM-co-St)@Bi2O3 composite hydrogel of mass content
Stress-strain curve.
Fig. 4 is P (AM-co-St)@Bi2O3Exterior view after the response of composite hydrogel laser.
Fig. 5 is P (AM-co-St)@Bi2O3The hole figure of composite hydrogel laser response region.
Fig. 6 is P (AM-co-St)@Bi2O3Hole internal structure chart after the response of composite hydrogel laser.
Specific embodiment
The present invention is described in further detail below with reference to embodiment, and each Example formulations are as shown in table 1.
The composition of raw materials of each embodiment of table 1 addition
Embodiment 1
It is formulated according to table 1, weighs AAm 6g, be dissolved in 15mL DMF, 0.15mL TMEDA is added as promotor, surpasses
0.2g St is added after sound oscillation 2min, MBA 0.12g is eventually adding 0.24g K2S2O8, 6h is reacted under the conditions of 25 DEG C, is obtained
To P (AM-co-St) hydrogel.The hydrogel of preparation is purified with deionized water later, changes a deionization every 8h
Water, purification is for 24 hours.
Using semiconductor laser marking, laser response test is directly carried out to P (AM-co-St) hydrogel, and observe
The optimum condition of its laser response performance.
Embodiment 2
It is formulated according to table 1, weighs AAm 6g, be dissolved in 15mL DMF, 0.15mL TMEDA is added as promotor, adds
Enter the modified Bi of 0.06g2O3, addition 0.2g St, MBA 0.12g is eventually adding 0.24g K to sonic oscillation 2min later2S2O8,
7h is reacted under the conditions of 25 DEG C, obtains P (AM-co-St)@Bi2O3Composite hydrogel.Later to the hydrogel deionization of preparation
Water is purified, and changes a deionized water every 8h, purification is for 24 hours.
The Bi of the modification2O3The preparation method comprises the following steps: measuring 40mL deionized water in 250mL beaker, the oxidation of 1g tri- two is added
Bismuth (Bi2O3), it stirs evenly, adds 0.2g3- (methacryloxypropyl) propyl trimethoxy silicane (TMSPMA), be put into oil bath
In pot, and oil bath temperature is increased to 70 DEG C, reacts 2h, obtains the modification Bi that end has double bond2O3Particle.
Using semiconductor laser marking, to P (AM-co-St)@Bi2O3Composite hydrogel directly carries out laser response and surveys
Examination, and observe the optimum condition of its laser response performance.
Embodiment 3
It is formulated according to table 1, weighs AAm 6g, be dissolved in 15mL deionized water, 0.15mL TMEDA is added as promotion
The modified Bi of 0.12g is added in agent2O3, addition 0.2g St, MBA 0.12g is eventually adding 0.24g to sonic oscillation 2min later
K2S2O8, 6h is reacted under the conditions of 25 DEG C, obtains P (AM-co-St)@Bi2O3Composite hydrogel.The hydrogel of preparation is used later
Deionized water is purified, and changes a deionized water every 8h, purification is for 24 hours.
The Bi of the modification2O3The preparation method comprises the following steps: measuring 40mL deionized water in 250mL beaker, the oxidation of 1g tri- two is added
Bismuth (Bi2O3), it stirs evenly, adds 0.2g 3- (methacryloxypropyl) propyl trimethoxy silicane (TMSPMA), be put into oil
In bath, and oil bath temperature is increased to 70 DEG C, reacts 2h, obtains the modification Bi that end has double bond2O3Particle.
Using semiconductor laser marking, to P (AM-co-St)@Bi2O3Composite hydrogel directly carries out laser response and surveys
Examination, and observe the optimum condition of its laser response performance.
Embodiment 4
It is formulated according to table 1, weighs AAm 6g, be dissolved in 15mL DMF, 0.15mL TMEDA is added as promotor, adds
Enter the modified Bi of 0.18g2O3, addition 0.2g St, MBA 0.12g is eventually adding 0.24g K to sonic oscillation 2min later2S2O8,
8h is reacted under the conditions of 25 DEG C, obtains P (AM-co-St)@Bi2O3Composite hydrogel.Later to the hydrogel deionization of preparation
Water is purified, and changes a deionized water every 8h, purification is for 24 hours.
The Bi of the modification2O3The preparation method comprises the following steps: measuring 40mL deionized water in 250mL beaker, the oxidation of 1g tri- two is added
Bismuth (Bi2O3), it stirs evenly, adds 0.2g3- (methacryloxypropyl) propyl trimethoxy silicane (TMSPMA), be put into oil bath
In pot, and oil bath temperature is increased to 70 DEG C, reacts 2h, obtains the modification Bi that end has double bond2O3Particle.
Using semiconductor laser marking, to P (AM-co-St)@Bi2O3Composite hydrogel directly carries out laser response and surveys
Examination, and observe the optimum condition of its laser response performance.
Comparative example 1
AAm 6g is weighed, is dissolved in 15mL deionized water, 0.15mL TMEDA is added as promotor, 0.12g is added not
Modified Bi2O3, MBA 0.12g is added after sonic oscillation 2min, is eventually adding 0.24g K2S2O8.6h is reacted at 25 DEG C,
Obtain PAM@Bi2O3Composite hydrogel.The hydrogel of preparation is purified with deionized water later, every 8h change once go from
Sub- water, purification is for 24 hours.Using semiconductor laser marking, laser response test is directly carried out to it, and observes the response of its laser
The optimum condition of performance
Comparative example 2
AAm 6g is weighed, is dissolved in 15mL DMF, 0.15mL TMEDA is added as promotor, 0.12g is added without changing
The Bi of property2O3, addition 0.2g St, MBA 0.12g is eventually adding 0.24g K to sonic oscillation 2min later2S2O8, in 25 DEG C of conditions
Lower reaction 6h obtains P (AM-co-St)@Bi2O3Composite hydrogel.The hydrogel of preparation is purified with deionized water later,
A deionized water is changed every 8h, purification is for 24 hours.Using semiconductor laser marking, laser response test is directly carried out to it,
And observe the optimum condition of its laser response performance
Comparative example 3
Polystyrene (PS) physics is first coated into Bi2O3, obtain PS@Bi2O3Compound particle, then AAm 6g is weighed, it is dissolved in
In 15mL DMF, 0.15mL TMEDA is added as promotor, 0.12g PS@Bi is added2O3Compound particle, sonic oscillation 2min
MBA 0.12g is added later, is eventually adding 0.24g K2S2O8, 7h is reacted under the conditions of 25 DEG C, obtains PAM/PS@Bi2O3It is compound
Hydrogel.The hydrogel of preparation is purified with deionized water later, changes a deionized water every 8h, purification is for 24 hours.
Comparative example 4
AAm 6g is weighed, is dissolved in 15mL DMF, 0.15mL TMEDA is added as promotor, 0.2g St, ultrasound is added
It vibrates 2min and 0.24g K is added later2S2O8, 8h is reacted at 60 DEG C, is obtained obtaining styrene/polyacrylamide copolymer, is added
0.12g non-modified Bi2O3, MBA 0.12g reacts 8h at 25 DEG C, obtains PAM/PS@Bi2O3Composite hydrogel.It is right later
The hydrogel of preparation is purified with deionized water, changes a deionized water every 8h, purification is for 24 hours.
Using semiconductor laser marking, laser response test is directly carried out to the composite hydrogel of preparation, and observe
The optimum condition of its laser response performance.
Pass through P (AM-co-St) hydrogel and P (AM-co-St)@Bi that Examples 1 to 4 is prepared2O3Compound water congealing
Glue carries out hydrophily detection, obtains physical parameter as shown in Table 2.
Table 2 P (AM-co-St)@Bi2O3The angle of wetting of composite hydrogel
Pass through P (AM-co-St) hydrogel and P (AM-co-St)@Bi that Examples 1 to 4 is prepared2O3Compound water congealing
Hydrogel prepared by glue and comparative example 1~4 carries out laser response test, acquired results such as table 3:
3 laser of table responds effect
Table 2 is the angle of wetting of Examples 1 to 4 hydrogel.As can be seen from the table, modified Bi is added2O3Compound particle it
Afterwards, the hydrophily of hydrogel is slightly decreased, this is because modified Bi2O3Compound particle is a kind of hydrophobic granule.
Table 3 is the laser response effect of Examples 1 to 4 and comparative example 1~4.As can be seen that adding in comparative example 1 in table 3
Non-modified Bi is entered2O3, obtain PAM@Bi2O3Composite hydrogel, laser effect are general；In comparative example 2, it joined not
Modified Bi2O3, it is prepared for P (AM-co-St)@Bi2O3Composite hydrogel, same laser effect are general；In comparative example 3, first
PS physics cladding Bi is prepared2O3Compound particle, then synthesize PAM/PS@Bi2O3Composite hydrogel, laser effect are general.Comparison
In example 4, the styrene/polyacrylamide copolymer first synthesized has added unmodified Bi2O3, laser effect is general.It is right
The general reason of 1~4 laser effect of ratio is Bi2O3Particle belongs to physical dispersion in hydrogel, and uniformity is bad, causes
Laser effect is general.In contrast, in Examples 1 to 4,3% modification Bi is added2O3Composite hydrogel to laser effect imitate
Fruit is most ideal, and modified Bi is not added in embodiment 12O3, hydrogel is responded without laser substantially, this is because in P (AM-co-St)
There is no the particles of laser response.Embodiment 2,3 and 4 has laser response, and embodiment 3 and 4 laser of embodiment response effect
Fruit is preferable, this is because wherein joined the Bi for having response to laser2O3Particle.Compared with comparative example, modified Bi is added2O3
Particle and then synthesis composite hydrogel, are combined by radical polymerization, and more uniform and stable system is dispersed,
Therefore laser response effect is ideal.
Fig. 4~6 are P (AM-co-St) the@Bi of embodiment 42O3Composite hydrogel SEM figure, after observing the response of its laser
Surface topography.Fig. 4 is observed, there are many apertures after the response of hydrogel surface laser, and surface bulge object may be PS@Bi2O3Compound grain
Son；Shown in Fig. 5, high magnification observes the hole of response region, and the network structure of discovery laser response water gel can be destroyed, and has new
Macropore occur.Its reason may be that hydrogel is tridimensional network, in laser response process, Bi2O3Being decomposed, it is black to generate
Color Bi simple substance, polystyrene are carbonized, so that PS@Bi2O3Compound particle is reduced, and hydrogel surface structure is destroyed, and hydrogel
In moisture evaporation, so there is biggish hole.Shown in Fig. 6, the internal structure of black hole is observed, is gone back inside discovery hole
There are many small holes, this also demonstrates the three-dimensional net structure of hydrogel.
Claims (6)
1. a kind of P (AM-co-St)@Bi of laser response2O3The preparation method of composite hydrogel, which is characterized in that the system
Preparation Method are as follows:
Step (1): solvent is measured in beaker, bismuth oxide (Bi is added2O3), it stirs evenly, adds 3- (metering system
Acyl-oxygen) propyl trimethoxy silicane (TMSPMA), oil bath temperature is increased to 70 DEG C, 2h is reacted, collects product after reaction, will produce
Object is placed in 60 DEG C of vacuum drying oven and is dried, and is ground after drying, and the modification Bi that end has double bond is obtained2O3Particle；
Step (2): acrylamide (AAm) is principal monomer, is dissolved in solvent, the styrene (St) for having double bond is added, then
The modification Bi that step (1) end has double bond is added again2O3Particle, and promotor, crosslinking agent and initiator is added, pass through freedom
Base polymerization preparation P (AM-co-St)@Bi2O3Composite hydrogel, later to the P of preparation (AM-co-St)@Bi2O3Composite hydrogel
It is purified, changes primary purification solution every 8h, purification is for 24 hours.
2. P (AM-co-St) the@Bi of laser response as described in claim 12O3The preparation method of composite hydrogel, feature
Be: acrylamide (AAm) the monomer structure formula is as follows:
The structural formula of the styrene (St) is as follows:
The structural formula of 3- (methacryloxypropyl) propyl trimethoxy silicane (TMSPMA) is as follows:
3. P (AM-co-St) the@Bi of laser response as described in claim 12O3The preparation method of composite hydrogel, feature
It is: TMSPMA and Bi described in step (1)2O3Mass ratio be 1:5.
4. P (AM-co-St) the@Bi of laser response as described in claim 12O3The preparation method of composite hydrogel, feature
Be: promotor described in step (2) is N, N, N ', N '-tetramethylethylenediamine (TMEDA) is；Crosslinking agent is N, N '-methylene
Bisacrylamide (MBA)；Initiator is potassium peroxydisulfate (K2S2O8)；The AAm, St, modified Bi2O3、TMEDA、MBA、K2S2O8's
Mass ratio is 50:1~3:0~3:1~2:1~2:1~3, and polymeric reaction temperature is 25 DEG C, and polymerization reaction time is 6~8h.
5. P (AM-co-St) the@Bi of laser response as described in claim 12O3The preparation method of composite hydrogel, feature
Be: in the step (1), solvent is deionized water；In step (2), solvent be n,N-Dimethylformamide (DMF) or go from
Sub- water, the solution of purification are deionized water.
6. a kind of P (AM-co-St) the@Bi of the response of laser made from preparation method as described in any one in claim 1-52O3It is multiple
Application of the Heshui gel in laser labelling, laser anti-counterfeit, laser tracking field, it is characterised in that: the P (AM-co-
St)@Bi2O3Composite hydrogel is directly to carry out laser marking using semiconductor laser marking, and the current strength of mark is in 15A
~20A.
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| CHUNLIN LIU等: ""Recognition of laser-marked quick response codes on polypropylene surfaces"", 《POLYMER DEGRADATION AND STABILITY》 * |
| ZHENG CAO等: ""Laser-induced blackening on surfaces of thermoplastic polyurethane/BiOCl composites"", 《POLYMER DEGRADATION AND STABILITY》 * |
| 高亮: ""混合溶剂下制备苯乙烯/丙烯酰胺温敏性聚合凝胶"", 《科技资讯》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112831147A (en) * | 2019-11-22 | 2021-05-25 | 北京服装学院 | Color-changing particle and preparation method thereof |
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| CN109180961B (en) | 2021-03-23 |
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