阅读说明：本技术 一种超低收缩率的光纤用环氧树脂粘合胶及其制备方法 (Epoxy resin adhesive for optical fiber with ultralow shrinkage rate and preparation method thereof ) 是由 倪晓伟 张来庆 程晓楠 苟曲廷 于 2021-09-27 设计创作，主要内容包括：本发明公开了一种超低收缩率的光纤用环氧树脂粘合胶及其制备方法。所述超低收缩率的光纤用环氧树脂粘合胶包括以下重量份数的原料制备而成：丙烯酸酯30-50份、活性单体20-40份、环氧树脂50-100份、光引发剂1-10份、固化剂1-10份、促进剂1-5份、填料10-30份、偶联剂1-5份。制得的光纤用环氧树脂粘合胶具有固化速度快、粘结力强的特点,固化后的光纤环氧胶具有超低的收缩率。(The invention discloses an epoxy resin adhesive for an optical fiber with ultralow shrinkage and a preparation method thereof. The epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared from the following raw materials in parts by weight: 30-50 parts of acrylate, 20-40 parts of active monomer, 50-100 parts of epoxy resin, 1-10 parts of photoinitiator, 1-10 parts of curing agent, 1-5 parts of accelerator, 10-30 parts of filler and 1-5 parts of coupling agent. The prepared epoxy resin adhesive for optical fibers has the characteristics of high curing speed and strong bonding force, and the cured optical fiber epoxy adhesive has ultralow shrinkage rate.)

1. The epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is characterized by comprising the following raw materials in parts by weight: 30-50 parts of acrylate, 20-40 parts of active monomer, 50-100 parts of epoxy resin, 1-10 parts of photoinitiator, 1-10 parts of curing agent, 1-5 parts of accelerator, 10-30 parts of filler and 1-5 parts of coupling agent.

2. The ultra-low shrinkage epoxy adhesive paste according to claim 1, wherein the acrylate comprises at least one of bisphenol a epoxy acrylate and urethane acrylate.

3. The ultra-low shrinkage epoxy adhesive paste for optical fibers according to claim 1, wherein the reactive monomer comprises ethoxylated trimethylolpropane triacrylate.

4. The ultralow-shrinkage epoxy adhesive paste for optical fibers according to claim 1, wherein the epoxy resin comprises bisphenol a type epoxy resin and bisphenol F type epoxy resin.

5. The ultra-low shrinkage epoxy adhesive paste for optical fibers according to claim 1, wherein the photoinitiator comprises at least one of ethyl 2,4, 6-trimethylbenzoylphenylphosphonate, 2-hydroxy-2-methyl-1-phenylpropanone;

the curing agent comprises a modified fatty amine curing agent;

the accelerator comprises zinc isooctanoate;

the filler comprises ground calcium carbonate;

the coupling agent comprises any one of a silane coupling agent KH 550, a silane coupling agent KH 560 and a silane coupling agent KH 570.

6. A method for preparing the ultralow-shrinkage epoxy resin adhesive glue for the optical fiber according to any one of claims 1 to 5, wherein the method comprises the following steps:

(1) preliminarily mixing the liquid raw materials in parts by weight to obtain a mixed solution;

(2) mixing the mixed solution obtained in the step (1) with the powder raw materials in parts by weight to obtain a powder-liquid mixed material;

(3) and (3) fully dispersing and mixing the powder-liquid mixture obtained in the step (2) to obtain the epoxy resin adhesive for the optical fiber with ultralow shrinkage rate.

7. The preparation method of the ultralow-shrinkage epoxy resin adhesive cement for the optical fiber according to claim 6, wherein the ultralow-shrinkage epoxy resin adhesive cement for the optical fiber is prepared by using a powder-liquid mixing device, the powder-liquid mixing device comprises a blending chamber (1), the blending chamber (1) is connected with a liquid spraying component and a powder spraying component, the powder spraying component is used for spraying powder into the blending chamber (1), and the liquid spraying component is used for atomizing a mixed liquid at the lower part of the blending chamber (1) to be instantly blended with a powder raw material sprayed by the powder spraying component;

the mixing assembly is used for mixing powder-liquid mixture obtained by mixing and melting in the mixing chamber (1), and comprises a mixing bin (2), wherein an impact pipe (3) is clamped in the middle of the upper surface of the mixing bin (2), and the mixing bin (2) is communicated with the mixing chamber (1) through the impact pipe (3);

impact assembly, fixed mounting be in mix the lower surface middle part of feed bin (2), it is right to mix the powder-liquid mixture in feed bin (2) and discharge and follow the both sides slope of impact pipe (3) is strikeed and is poured into, the liquid jet subassembly includes water pump (6), the delivery port fixed mounting of water pump (6) has notes liquid pipe (10), it has injection post (11) to annotate liquid pipe (10) fixed mounting, injection post (11) run through and fixed connection in the top of handing over and melting room (1), fixed and the intercommunication of injection post (11) have injection dish (12), a plurality of shower nozzles (13) have been seted up on injection dish (12), shower nozzle (13) are the setting of multirow arc.

Technical Field

The invention belongs to the technical field of adhesives, and particularly relates to an epoxy resin adhesive for an optical fiber with ultralow shrinkage and a preparation method thereof.

Background

The optical fiber material needs to be fixedly connected through an optical fiber connecting machine by using adhesive glue, the adhesive glue for the optical fiber generally adopts epoxy glue, and the connecting material of the epoxy glue is light-cured resin or thermosetting resin or both. The polymerization reaction in the resin curing process can bring about the change of interatomic distance, so that the volume shrinkage of the epoxy glue occurs, and the volume shrinkage of the epoxy glue not only influences the size precision of bonding, but also can cause the reduction of bonding force.

Therefore, the research on the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate reduces or even eliminates the volume shrinkage in the curing process, and has important significance for improving the size precision and the bonding strength of the bonded optical fiber.

The curing shrinkage of the adhesive can be effectively reduced by adopting low-viscosity oligomer and adding inert inorganic filler, but the wettability of the inert inorganic filler and a polymer is poor, and the dispersion degree of the inert inorganic filler in a polymer system needs to be improved so as to obtain a product with uniform components and stable quality.

Disclosure of Invention

Based on the defects in the prior art, the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is provided, and has the characteristics of high curing speed and strong bonding force, and the cured optical fiber epoxy adhesive has the ultralow shrinkage rate.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared from the following raw materials in parts by weight: 30-50 parts of acrylate, 20-40 parts of active monomer, 50-100 parts of epoxy resin, 1-10 parts of photoinitiator, 1-10 parts of curing agent, 1-5 parts of accelerator, 10-30 parts of filler and 1-5 parts of coupling agent.

Preferably, the acrylate comprises at least one of bisphenol a type epoxy acrylate and urethane acrylate.

Preferably, the reactive monomer comprises ethoxylated trimethylolpropane triacrylate.

Preferably, the epoxy resin includes bisphenol a type epoxy resin and bisphenol F type epoxy resin;

preferably, the weight ratio of the bisphenol A type epoxy resin to the bisphenol F type epoxy resin is 1-3: 1;

preferably, the photoinitiator comprises at least one of ethyl 2,4, 6-trimethylbenzoylphenylphosphonate (photoinitiator TPO-L), 2-hydroxy-2-methyl-1-phenylpropanone (photoinitiator 1173);

the curing agent comprises a modified fatty amine curing agent;

the modified fatty amine curing agent comprises a curing agent 593 (an adduct of diethylenetriamine and butyl glycidyl ether);

the accelerator comprises zinc isooctanoate;

preferably, the filler comprises ground calcium carbonate;

the coupling agent comprises any one of a silane coupling agent KH 550, a silane coupling agent KH 560 and a silane coupling agent KH 570.

A preparation method of epoxy resin adhesive for optical fibers with ultralow shrinkage rate comprises the following steps:

(1) preliminarily mixing the liquid raw materials in parts by weight to obtain a mixed solution;

(2) mixing the mixed solution obtained in the step (1) with the powder raw materials in parts by weight to obtain a powder-liquid mixed material;

(3) and (3) fully dispersing and mixing the powder-liquid mixture obtained in the step (2) to obtain the epoxy resin adhesive for the optical fiber with ultralow shrinkage rate.

Compared with the prior art, the invention has the following beneficial effects:

1. the epoxy resin adhesive for the optical fiber prepared by the invention comprises UV curing and thermocuring dual curing components, wherein the epoxy resin in the thermocuring component mainly adopts bisphenol A type epoxy resin with small volume shrinkage during curing, and a filler is added as an anti-shrinkage agent to provide a rigid framework or support for the epoxy resin and reduce the shrinkage rate of the resin, so that the prepared epoxy resin adhesive for the optical fiber has ultralow shrinkage rate after curing, and the dual curing components enable the epoxy resin to have high curing speed and strong binding power.

2. The epoxy resin disclosed by the invention comprises bisphenol F type epoxy resin besides bisphenol A type epoxy resin, and the bisphenol F type epoxy resin has low viscosity, so that the viscosity of the epoxy adhesive can be reduced, and the foaming property of the epoxy adhesive can be reduced; the impregnability to the filler is good, and the compatibility of the epoxy adhesive and the filler is improved; the condensate has better comprehensive performance and has good heat resistance and water resistance with the bisphenol A type blended epoxy resin.

3. In the invention, except for the filler heavy calcium carbonate as a powder raw material, other raw materials are liquid raw materials, and the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared by adopting a powder-liquid mixing device, the preparation process is easy to operate and realize, so that the liquid raw materials can be fully dispersed and uniformly mixed, the powdery filler can be fully dispersed and infiltrated in the liquid raw materials, and the prepared adhesive has uniform components and stable properties, and has good adhesive performance when being used as an adhesive for the optical fiber.

Drawings

FIG. 1 is a flow diagram of a manufacturing process of the present invention;

FIG. 2 is a perspective view of a powder-liquid mixing device according to the present invention;

FIG. 3 is a second perspective view of the powder-liquid mixing device according to the present invention;

FIG. 4 is a view showing the internal structure of the powder-liquid mixing apparatus according to the present invention;

FIG. 5 is an exploded view of the powder-liquid mixing device of the present invention;

FIG. 6 is a third perspective view of the powder-liquid mixing device of the present invention.

In the figure: 1. a blending chamber; 2. a mixing bin; 3. an impingement tube; 4. a base; 5. a foot pad; 6. a water pump; 7. a mixing tube; 8. a shunt tube; 9. a flow meter; 10. a liquid injection pipe; 11. a spray column; 12. a spray tray; 13. a spray head; 14. a powder box; 15. a hose; 16. a powder spray gun; 17. a stirring wheel; 18. a first bevel gear; 19. a second bevel gear; 20. a gear shaft; 21. a transmission case; 22. a motor; 23. a discharge pipe; 24. a first electromagnetic valve; 25. a four-way connector; 26. injecting into a branch pipe; 27. an impingement tank; 28. an injection header pipe; 29. an impact piston; 30. a piston rod; 31. a double-shaft cylinder; 32. a discharge pipe; 33. a third electromagnetic valve; 34. and a second electromagnetic valve.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared from the following raw materials in parts by weight: 30 parts of bisphenol A epoxy acrylate, 20 parts of ethoxylated trimethylolpropane triacrylate, 25 parts of bisphenol A epoxy resin, 25 parts of bisphenol F epoxy resin, 1 part of photoinitiator TPO-L, 5931 parts of curing agent, 1 part of zinc isooctanoate, 10 parts of heavy calcium carbonate and 1 part of silane coupling agent KH 5501 parts;

the preparation method comprises the following steps:

(1) preliminarily mixing bisphenol A epoxy acrylate, ethoxylated trimethylolpropane triacrylate, bisphenol A epoxy resin, bisphenol F epoxy resin, a photoinitiator TPO-L, a curing agent 593, zinc isooctanoate and a silane coupling agent KH 550 in parts by weight to obtain a mixed solution;

(2) mixing the mixed solution obtained in the step (1) with heavy calcium carbonate in parts by weight to obtain a powder-liquid mixed material;

(3) and (3) fully dispersing and mixing the powder-liquid mixture obtained in the step (2) to obtain the epoxy resin adhesive for the optical fiber with ultralow shrinkage rate.

Example 2

The epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared from the following raw materials in parts by weight: 50 parts of urethane acrylate, 40 parts of ethoxylated trimethylolpropane triacrylate, 75 parts of bisphenol A epoxy resin, 25 parts of bisphenol F epoxy resin, 117310 parts of photoinitiator, 59310 parts of curing agent, 10 parts of zinc isooctanoate, 30 parts of heavy calcium carbonate and 5605 parts of silane coupling agent KH;

the preparation method comprises the following steps:

(1) preliminarily mixing bisphenol A epoxy acrylate, ethoxylated trimethylolpropane triacrylate, bisphenol A epoxy resin, bisphenol F epoxy resin, a photoinitiator 1173, a curing agent 593, zinc isooctanoate and a silane coupling agent KH 560 according to parts by weight to obtain a mixed solution;

(2) mixing the mixed solution obtained in the step (1) with heavy calcium carbonate in parts by weight to obtain a powder-liquid mixed material;

(3) and (3) fully dispersing and mixing the powder-liquid mixture obtained in the step (2) to obtain the epoxy resin adhesive for the optical fiber with ultralow shrinkage rate.

Example 3

The epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared from the following raw materials in parts by weight: 20 parts of bisphenol A epoxy acrylate, 20 parts of urethane acrylate, 30 parts of ethoxylated trimethylolpropane triacrylate, 50 parts of bisphenol A epoxy resin, 25 parts of bisphenol F epoxy resin, 2.5 parts of photoinitiator TPO-L, 11732.5 parts of photoinitiator, 5935 parts of curing agent, 3 parts of zinc isooctanoate, 20 parts of heavy calcium carbonate and KH 5703 parts of silane coupling agent;

the preparation method comprises the following steps:

(1) preliminarily mixing bisphenol A epoxy acrylate, urethane acrylate, ethoxylated trimethylolpropane triacrylate, bisphenol A epoxy resin, bisphenol F epoxy resin, a photoinitiator TPO-L, a photoinitiator 1173, a curing agent 593, zinc isooctanoate and a silane coupling agent KH570 in parts by weight to obtain a mixed solution;

(2) mixing the mixed solution obtained in the step (1) with heavy calcium carbonate in parts by weight to obtain a powder-liquid mixed material;

(3) and (3) fully dispersing and mixing the powder-liquid mixture obtained in the step (2) to obtain the epoxy resin adhesive for the optical fiber with ultralow shrinkage rate.

In examples 1 to 3, bisphenol A type epoxy acrylate was supplied by Germany good chemical company, Inc. (China), Cat No.: RJ 313; urethane acrylate is supplied by good chemical company (china) ltd, germany, a cargo number: RJ 4239; bisphenol a type epoxy resin is supplied by the tomb petrochemical, cargo number: CYD-128; bisphenol F type epoxy resins are supplied by hansen HEXION, usa, cat #: epikote 862.

Comparative example 1

Compared with example 1, in comparative example 1, no filler ground calcium carbonate was added, and other conditions were unchanged.

Comparative example 2

Compared with example 1, in comparative example 1, no silane coupling agent KH 550 was added, and other conditions were not changed.

Comparative example 3

Compared with the example 1, in the comparative example 1, the epoxy resin adhesive glue for the optical fiber with the ultralow shrinkage rate is prepared without adopting a powder-liquid mixing device, after the liquid raw materials are mixed in a reaction kettle, the ground limestone is added into the mixed liquid, the stirring and the dispersion are continued, and the processing time is the same as the time for preparing by adopting the powder-liquid mixing device.

Example 4

This example discloses a powder-liquid mixing device, in which the preparation of the epoxy adhesive paste for optical fiber with ultra-low shrinkage rate in the above examples 1-3 was carried out.

As shown in fig. 2 to 6, the powder-liquid mixing device includes an blending component, which includes a blending chamber 1, the blending chamber 1 is connected to a liquid spraying component and a powder spraying component, the powder spraying component is used for spraying powder into the blending chamber 1, the liquid spraying component is used for atomizing a mixed liquid at the lower part of the blending chamber 1 to blend with a powder raw material sprayed by the powder spraying component instantaneously;

the mixing assembly is used for mixing powder-liquid mixture obtained by blending and melting in the blending chamber 1 and comprises a mixing bin 2, an impact pipe 3 is clamped in the middle of the upper surface of the mixing bin 2, and the mixing bin 2 is communicated with the blending chamber 1 through the impact pipe 3;

and the impact assembly is fixedly arranged in the middle of the lower surface of the mixing bin 2 and is used for discharging the powder-liquid mixture in the mixing bin 2 and injecting the powder-liquid mixture from two sides of the impact pipe 3 in an inclined impact manner.

Still include base 4, the last fixed surface of base 4 installs powder injection subassembly, liquid injection subassembly and impact the subassembly, impact the subassembly with parallel arrangement around powder injection subassembly and liquid injection subassembly are, the lower surface four corners fixed mounting of base 4 has pad foot 5

Further, the liquid injection assembly comprises a water pump 6, a mixing pipe 7 is fixedly installed at a water inlet of the water pump 6, a plurality of shunt pipes 8 are arranged on the mixing pipe 7, flow meters 9 are installed on the shunt pipes 8, the shunt pipes 8 are used for being externally connected with feeding devices of all liquid raw materials, and the feeding devices corresponding to all the liquid raw materials are gradually decreased relative to the water pump 6 according to the required amount of all the liquid raw materials and are distributed from far to near;

the delivery port fixed mounting of water pump 6 has notes liquid pipe 10, it has injection post 11 to annotate liquid pipe 10 fixed mounting, injection post 11 runs through and fixed connection in the top of blending room 1, injection post 11 is fixed and the intercommunication has injection dish 12, a plurality of shower nozzles 13 have been seted up on injection dish 12, shower nozzle 13 is the setting of multirow arc.

The powder spraying assembly comprises a powder box 14, a powder spraying gun 16 is fixedly installed on the powder box 14 through a hose 15, and the powder spraying gun 16 is fixedly installed on one side of the inner wall of the blending chamber 1.

So that the liquid raw materials are respectively injected into the mixing pipe 7 according to the proportion to achieve the primary mixing of the liquid raw materials to form mixed liquid, then the mixed liquid is injected into the injection column 11 through the liquid injection pipe 10 by the water pump 6, thereby forming a mixed liquid water curtain in the melting chamber 1 through the injection tray 12 and the spray head 13, then the powder raw material in the powder box 14 is sprayed out through the powder spray gun 16, so that the powder raw material is rapidly dispersed and mutually blended with the mixed liquid water curtain when being sprayed out, so as to lead the powder raw material and the mixed liquid to achieve the preliminary mixing, instantaneously combine and match with the multi-row arc arrangement of the spraying disc 12 and the spray head 13 to form a multi-layer mixed liquid water curtain, therefore, the powder raw materials and the mixed liquid are directly dropped after being mixed, the powder raw materials can be effectively prevented from flying, and air pollution caused by flying dust is avoided on the basis of primary mixing.

The spray head 13 can spray the mixed liquid in a water flow state or a water mist state, but when spraying the water mist, the particle size of water drops in the water mist needs to be controlled, the water mist flows downwards after being sprayed, and the phenomenon that the water mist is combined with the powder raw material and then flows upwards to adhere to the spray tray 12 to cause serious difference in the proportion of the powder raw material is avoided;

the liquid raw material feeding device externally connected with the shunt pipe 8 comprises a liquid tank for containing raw materials and an extraction pump, and the water outlet of the extraction pump is in butt joint with the shunt pipe 8;

the distribution principle of the feeding device is as follows: assuming that there are three liquid raw materials, A, B, C, 1 part of liquid raw material A, 2 parts of liquid raw material B and 3 parts of liquid raw material C, the feeding device corresponding to the liquid raw material C is in butt joint with the shunt pipe 8 farthest from the water pump 6, the feeding device corresponding to the liquid raw material A is in butt joint with the shunt pipe 8 nearest to the water pump 6, and the feeding device corresponding to the liquid raw material B is in butt joint with the shunt pipe in the shunt pipes 8 in butt joint with the feeding devices corresponding to the liquid raw materials A and C.

Further, the inner wall one side symmetry of mixing feed bin 2 runs through and the swivelling joint has a stirring wheel 17, the pivot of stirring wheel 17 runs through 2 fixed mounting in mixing feed bin has helical gear 18, the meshing of helical gear 18 has helical gear two 19, helical gear two 19 run through and fixedly connected with gear shaft 20, gear shaft 20 runs through and rotates and is connected with transmission case 21, transmission case 21 fixed mounting be in mix one side of feed bin 2, gear shaft 20 fixed mounting has motor 22, motor 22 fixed mounting be in one side of transmission case 21 is used for passing through helical gear 18 and the drive of helical gear two 19 the reverse relative rotation of stirring wheel 17.

The motor 22 drives the gear shaft 20 to rotate, the gear shaft 20 drives the second bevel gear 19 to rotate, and the second bevel gear 19 drives the first bevel gear 18 to rotate in the opposite direction through the meshing of the second bevel gear 19 and the first bevel gear 18, so that the stirring wheel 17 realizes the opposite rotation in the stirring bin 2, and the powder-liquid mixture entering the stirring bin 2 is fully stirred; through the reverse relative rotation of stirring wheel 17, make the powder liquid mixture of both sides stir between stirring wheel 17 under the effect of stirring wheel 17 to form the striking, further strengthen mixing intensity, make intensive mixing dispersion between powder raw materials and the liquid raw materials, also further make intensive mixing between each liquid raw materials simultaneously, through the mutual striking of the powder liquid mixture of both sides, make the bubble that contains inside break, thereby obtain eliminating.

Further, the material discharging pipe 23 is arranged in the middle of the lower surface of the material mixing bin 2, the first electromagnetic valve 24 is arranged on the material discharging pipe 23, and the material discharging pipe 23 is connected with an impact assembly.

Thereby before mixing feed bin 2 is poured into completely at raw materials mixed liquid and powder raw materials, through closing solenoid valve 24, make powder liquid mixture stop completely in mixing feed bin 2 and carry out the preliminary defoaming, the preliminary defoaming and the purpose of mixing through stirring wheel 17, mix after feed bin 2 is mixed liquid and powder raw materials and pour into completely, open solenoid valve 24 and solenoid valve two 34, close solenoid valve three 33 simultaneously, make the mixed liquid of powder liquid get into the impact subassembly.

Further, strike the subassembly and include four-way connection head 25, arrange row material pipe 23 fixedly connected with the upper end of four-way connection head 25, four-way connection head 25's both sides fixed mounting has injection branch pipe 26, two 34 solenoid valves have all been seted up on the injection branch pipe 26, the one end fixedly connected with of injection branch pipe 26 strikes jar 27, just injection branch pipe 26 with strike jar 27 intercommunication, the one end of striking jar 27 is connected with and pours into house steward 28, pour into house steward 28 with strike 3 fixed and the intercommunication of pipe, install the impact element in the jar 27 of striking.

The impact element comprises an impact piston 29, the impact piston 29 is in sliding connection with the inner wall of the impact tank 27, a piston rod 30 is installed at one end of the impact piston 29, the piston rod 30 penetrates through and is in sliding connection with the impact tank 27, a double-shaft cylinder 31 is fixedly connected to one end of the piston rod 30, and the double-shaft cylinder 31 is fixedly installed in the middle of one side of the upper surface of the base 4.

Therefore, the powder and liquid enter the impact tank 27 through the injection branch pipe 26, then along with the output of the double-shaft cylinder 31, the output shaft of the double-shaft cylinder 31 drives the impact piston 29 to extrude the powder and liquid mixture through the piston rod 30, and further the powder and liquid mixture enters the impact pipe 3 through the injection main pipe 28, and as the connectors with inclined and symmetrical inlets are arranged at the two sides of the impact pipe 3, the mixed powder and liquid forms counter impact when entering the impact pipe 3 from the connectors, so that the powder and liquid are further mixed, and simultaneously defoaming treatment is carried out, and the requirement of uniform dispersion of the powder and liquid is met;

when the impact piston 29 impacts the powder-liquid mixture, the impact piston 29 blocks a connecting port of the injection branch pipe 26 and the impact tank 27, so that the powder-liquid mixture is prevented from entering one end of the injection main pipe 28 of the impact tank 27, after the impact piston 29 is reset, the connecting port of the injection branch pipe 26 and the impact tank 27 is opened again, and after the powder-liquid flows in, the powder-liquid mixture is impacted and extruded through the double-shaft cylinder 31 again.

Further, the lower end of the four-way connector 25 is connected with a discharge pipe 32, and the discharge pipe 32 is provided with a third electromagnetic valve 33.

After powder and liquid after impact enter the mixing bin 2, impact treatment is carried out again, after the process is circulated for a plurality of times, the first electromagnetic valve 24 is closed, powder does not enter the mixing bin 2 after impact, after the powder completely enters the mixing bin again, the second electromagnetic valve 34 is closed, the first electromagnetic valve 24 and the third electromagnetic valve 33 are opened, the powder and liquid mixture is discharged from the discharge pipe 32, and uniform dispersion and mixing of various liquid raw materials and powder raw materials in epoxy resin adhesive preparation are completed.

When in use, the steps are as follows:

s1: powder raw materials are placed in a powder box 14 according to parts by weight, the liquid raw materials are respectively injected into a mixing pipe 7 according to parts by weight through a shunt pipe 8 to achieve preliminary mixing of the liquid raw materials to form mixed liquid, then the mixed liquid is injected into a spray column 11 through a liquid injection pipe 10 through a water pump 6, so that a mixed liquid water curtain is formed in a blending chamber 1 through a spray disc 12 and a spray head 13, then the powder raw materials in the powder box 14 are sprayed out through a powder spray gun 16, so that the powder raw materials are quickly scattered and mutually blended with the mixed liquid water curtain when being sprayed, the powder raw materials and the mixed liquid achieve preliminary mixing to form a powder-liquid mixed material, multiple rows of arcs of the spray disc 12 and the spray head 13 are instantaneously combined and matched to form multiple layers of mixed liquid water curtains, the powder raw materials and the mixed liquid directly fall down after being mixed, and the powder raw materials can be effectively prevented from flying, thereby avoiding air pollution caused by dust flying on the basis of primary mixing;

s2: the powder-liquid mixture enters the mixing bin, the first electromagnetic valve 24 is closed at the moment, the gear shaft 20 is driven to rotate through the motor 22, the second bevel gear 19 is driven to rotate through the gear shaft 20, and further the bevel gear 19 is meshed with the bevel gear 18, so that the bevel gear 19 drives the bevel gear 18 to rotate in the opposite direction, the mixing wheel 17 is enabled to rotate in the mixing bin 2 in the opposite direction, and the powder-liquid mixture entering the mixing bin 2 is fully mixed; through the reverse relative rotation of the stirring wheel 17, the powder-liquid mixture on the two sides is stirred between the stirring wheels 17 under the action of the stirring wheels 17, so that impact is formed, the mixing strength is further enhanced, the powder raw material and the liquid raw material are fully mixed and dispersed, meanwhile, the liquid raw materials are fully mixed, and the powder-liquid mixture on the two sides impacts with each other to break bubbles contained in the powder-liquid mixture, so that the bubbles are eliminated;

s3: after the mixed liquid and the powder raw materials are completely injected into the mixing bin 2, opening the first electromagnetic valve 24 and the second electromagnetic valve 34, and simultaneously closing the third electromagnetic valve 33 to enable the powder-liquid mixed materials to enter the impact assembly;

s4: the powder-liquid mixture enters the impact tank 27 through the injection branch pipe 26, then along with the output of the double-shaft cylinder 31, the output shaft of the double-shaft cylinder 31 drives the impact piston 29 to extrude the powder-liquid mixture through the piston rod 30, and further the powder-liquid mixture enters the impact pipe 3 through the injection main pipe 28, and as connectors with inclined and symmetrical inlets are arranged at two sides of the impact pipe 3, the powder-liquid mixture forms hedging when entering the impact pipe 3 from the connectors, so that the further mixing is carried out, and simultaneously, the defoaming treatment is carried out, thereby meeting the requirement of uniform dispersion of the powder-liquid;

s5: after the powder-liquid mixture after impact enters the mixing bin 2, impact treatment is carried out again, after the process is circulated for a plurality of times, the first electromagnetic valve 24 is closed, the powder-liquid mixture continuously impacts and then enters the mixing bin 2, after the powder-liquid mixture completely enters the mixing bin again, the second electromagnetic valve 34 is closed, the first electromagnetic valve 24 and the third electromagnetic valve 33 are opened, the powder-liquid mixture is discharged from the discharge pipe 32, and uniform dispersion and mixing of various liquid raw materials and powder raw materials in epoxy resin adhesive preparation are completed.

Further, the liquid raw materials are respectively injected into the mixing pipe according to the weight portion to achieve the primary mixing of the liquid raw materials to form mixed liquid, then the mixed liquid is injected into the injection column through the liquid injection pipe by the water pump, thereby forming a mixed liquid water curtain in the blending chamber through the injection disc and the spray head, then the powder raw material in the powder box is sprayed out through a powder spray gun, so that the powder raw material is rapidly dispersed and mutually blended with the mixed liquid water curtain when being sprayed out, so that the powder raw material and the mixed liquid are preliminarily mixed to form a powder-liquid mixed material, and the powder-liquid mixed material is instantaneously combined and matched with a plurality of rows of arc-shaped arrangements of the spraying disc and the spray head to form a multi-layer mixed liquid water curtain, therefore, the powder raw materials and the mixed liquid are directly dropped after being mixed, the powder raw materials can be effectively prevented from flying, and air pollution caused by flying dust is avoided on the basis of primary mixing.

Further, the second bevel gear is driven to rotate by the gear shaft, and the first bevel gear is driven to rotate in the opposite direction by the second bevel gear through the meshing of the second bevel gear and the first bevel gear, so that the stirring wheel can rotate in the opposite direction in the stirring bin, and the powder-liquid mixture entering the stirring bin is fully stirred; through the reverse relative rotation of stirring wheel, make the powder liquid mixture of both sides stir between the stirring wheel under the effect of stirring wheel to form the striking, further reinforcing mixing intensity makes intensive mixing dispersion between powder raw materials and the liquid raw materials, also further makes intensive mixing between each liquid raw materials simultaneously, through the powder liquid mixture striking each other of both sides, makes the bubble that contains inside break, thereby obtains eliminating.

Further, through powder liquid mixture through pouring into the branch pipe and get into the impact jar, then along with the output of biax cylinder, the output shaft that makes the biax cylinder drives through the piston rod and strikes piston extrusion powder liquid mixture, and then make powder liquid mixture through pouring into the house steward and get into the impact pipe, because the both sides of impacting the pipe are provided with the connector of entry slope and symmetry, when powder liquid mixture gets into the impact pipe from the connector, form and dash, thereby further mix, carry out the defoaming simultaneously and handle, the requirement to the homodisperse of powder liquid mixture has been reached.

Examples of the experiments

The ultra-low shrinkage optical fibers prepared in the specific examples 1 to 3 and the comparative examples 1 to 3 were subjected to a performance test using an epoxy adhesive paste:

(1) and (3) determination of curing shrinkage: according to the provisions of Standard ISO 3521-1997 determination of the shrinkage of the total volume of unsaturated polyester and epoxy resin;

(2) and (3) testing the bonding strength: the tensile shear strength was determined according to the criteria in GB/T7124-.

The test results are shown in table 1:

TABLE 1

Test items	Curing shrinkage (%)	Tensile shear Strength (MPa)
			Example 1	0.37	13.8
Example 2	0.35	14.0
			Example 3	0.36	13.9
Comparative example 1	0.51	13.1
			Comparative example 2	0.39	12.8
Comparative example 3	0.43	13.3

The test results in table 1 show that the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate prepared by the invention has the characteristics of high bonding strength, low curing shrinkage rate and the like.

Compared with example 1, in comparative example 1, when the epoxy resin adhesive for optical fibers with ultralow shrinkage is prepared, no filler heavy calcium carbonate is added, and the prepared adhesive has larger shrinkage after curing due to lack of a rigid skeleton.

Compared with example 1, when the epoxy resin adhesive for optical fibers with ultralow shrinkage rate is prepared in comparative example 2, the silane coupling agent KH 550 is not added, the compatibility among raw materials is reduced, the bonding performance of the prepared adhesive is weakened, and the tensile shear strength is reduced.

Compared with the example 1, when the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared in the comparative example 3, the epoxy resin adhesive for the optical fiber with the ultralow shrinkage rate is prepared without adopting a powder-liquid mixing device, the materials are not sufficiently mixed and dispersed, the component uniformity of the adhesive is poor, and the bonding strength is reduced.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.