CN211098954U

CN211098954U - Device for preparing polyacrylamide nano microspheres by photo-initiation

Info

Publication number: CN211098954U
Application number: CN201921715561.4U
Authority: CN
Inventors: 汪希领; 丁金皓; 刘平; 马亚斌; 付立辉; 井军平; 李海斌
Original assignee: Xi'an Wonder Energy Chemical Co ltd
Current assignee: Xi'an Wonder Energy Chemical Co ltd
Priority date: 2019-10-14
Filing date: 2019-10-14
Publication date: 2020-07-28
Anticipated expiration: 2029-10-14

Abstract

The utility model provides a device for photoinitiation preparation polyacrylamide nanometer microballon belongs to polymer material preparation technical field. The device provided by the utility model comprises a light source, a dispersion prism and a multi-channel micro-tube reactor, wherein the multi-channel micro-tube reactor comprises a constant temperature box, a plurality of opaque baffles and a plurality of horizontal tube reactors, the opaque baffles and the horizontal tube reactors are arranged at intervals in the constant temperature box, the opaque baffles separate each horizontal tube reactor, and the horizontal tube reactors are made of transparent materials; the light dispersion surface of the dispersion prism is positioned above the multichannel micro-tube reactor.

Description

Device for preparing polyacrylamide nano microspheres by photo-initiation

Technical Field

The utility model relates to a polymer material preparation technical field especially relates to a device that is used for photoinitiation preparation polyacrylamide nanometer microballon.

Background

The polyacrylamide microsphere is also called cross-linked polymer microsphere, is a water-absorbent resin with wide application, and is mainly applied to deep profile control and water shutoff of oil fields with strong heterogeneity, high water content and large pore canal development. The polymer microspheres have the advantages of small size, good dispersibility in water, easiness in entering deep parts of stratums, water swelling at oil reservoir temperature and the like, and in the deep profile control and water plugging process, the polymer microspheres are enabled to move, plug, deform and pass in pore throats and then move to plug until the deep parts of the stratums, so that the water channeling dominant channels are plugged step by step, deep plugging is realized, and the oil recovery rate is further improved.

The method for preparing the polyacrylamide microspheres by photo-initiation has attracted attention in recent years, the photoinitiator is used, the activation energy is low, low-temperature polymerization is easy, the photoinitiator can be completely decomposed, the obtained product does not contain initiator residues, the purity is relatively high, and most importantly, the microspheres obtained by photo-initiation polymerization have better dispersibility and narrower particle size distribution width. The prior art CN 103965396A discloses a radiation polymerization method for preparing polyacrylamide polymer gel microspheres, and relates to a radiation polymerization array device, a radiation source used in the method belongs to a dangerous substance, the array device is intermittent, and external forces such as stirring, vibration, rotation and the like are applied to disperse materials; the prior art CN 101555298A discloses a preparation method for controlling the molecular weight of a polymer by heterogeneous continuous photopolymerization, which continuously flows a mixed solution consisting of a monomer, an initiator and a solvent into a reactor at a certain flow rate, and is solidified under a certain temperature and illumination condition, and the polymer is obtained by heterogeneous precipitation, the method cannot continuously produce, and the product needs to be separated in the reactor, the solidified polymer is easily adhered to the wall of the reactor, and the product is difficult to separate; the prior art CN 109289723A discloses a device of photopolymerization microchannel, and the method utilizes the focusing and reflection of light to make the raw materials obtain sufficient illumination in the device, thereby generating polymerization reaction. In addition, the method has high requirements on the light source, and the light source has great harm to human bodies, thus being not beneficial to industrial application.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to provide a device for photoinitiation preparation polyacrylamide nanometer microballon, the utility model provides a device simple structure easily controls, and when preparation polyacrylamide nanometer microballon, requires lowly to the light source, is fit for the industrialization and uses.

In order to realize the purpose of the utility model, the utility model provides a following technical scheme:

the utility model provides a device for photoinitiation preparation polyacrylamide nanometer microballon, including light source, dispersion prism and multichannel microtube reactor, the multichannel microtube reactor includes thermostated container, a plurality of opaque baffle and a plurality of horizontal tubular reactor, opaque baffle and horizontal tubular reactor interval arrangement in the thermostated container, and opaque baffle separates each horizontal tubular reactor, the material of horizontal tubular reactor is transparent material; the light dispersion surface of the dispersion prism is positioned above the multichannel micro-tube reactor.

Preferably, the device for preparing the polyacrylamide nano-microspheres by photoinitiation further comprises a light source control box for controlling the on-off of the light source and the intensity of the light source.

Preferably, the device for preparing the polyacrylamide nano-microspheres by photoinitiation further comprises a light source and a prism height adjusting box, and the light source and the prism height adjusting box are used for adjusting the heights of the light source and the dispersion prism.

Preferably, the light source is disposed in the light source box, the dispersion prism is disposed in the prism box, and a shading box is disposed between the light source box and the prism box.

Preferably, a closed box is arranged above the multi-channel micro-tube reactor, and the prism box is positioned above the closed box.

Preferably, the dispersion prism is a dispersion triple prism or a dispersion quadruple prism, and the refractive index of the dispersion prism is 1.210-1.580.

Preferably, the inner diameter of the horizontal tubular reactor is 20-38 mm, the total length is 20-80 m, and the horizontal length of the horizontal tubular reactor is 50-80 cm; the length of the light dispersion surface of the dispersion prism is 100-300 mm.

Preferably, the constant temperature box is a constant temperature water bath box.

Preferably, a feed inlet of the horizontal tubular reactor is communicated with the raw material mixing kettle through a pipeline, and a material pump is arranged on the pipeline.

Preferably, the discharge port of the horizontal tubular reactor is provided with a product collector.

The device provided by the utility model requires lowly to the light source, adopt the visible light source can, the security has obtained very big improvement, and after dispersion prism dispersion, can produce different typefaces, the wavelength range that each typeface corresponds is different, and be provided with opaque baffle between the horizontal tubular reactor that corresponds with the typeface, the interference between different typefaces has been avoided, can suitably adjust the photoinitiator type and content in the liquid stream of acrylamide in each pipeline according to this, realize the control to polymerization reaction rate and reaction degree in each pipeline, preparation required product; moreover, because the reactor of the utility model is a multi-channel micro-tube reactor, products with different particle sizes can be obtained at one time through each horizontal tube reactor, or products with the same particle size can be obtained by changing the dosage or the type of the initiator, thereby not only improving the product quality and the production efficiency, but also reducing the production cost; in addition, the device provided by the utility model can be used for continuous production.

Furthermore, the visible light source acts on the upper part of the horizontal tubular reactor, the irradiation intensity of the visible light source is basically consistent with the advancing direction of the materials, the decomposition speed of the photoinitiator also presents the trend of first-speed and second-speed along with the gradual decrease of the light source intensity from top to bottom, is consistent with the dynamic characteristic of polymerization characteristic of acrylamide, namely 'fast initiation, fast growth and slow termination', meanwhile, because the material of the horizontal tubular reactor is transparent material and the water bath in the constant temperature box and the material in the pipeline are basically transparent, therefore, the light of each color band can fill a single pipeline (namely a horizontal tubular reactor) from strong to weak from top to bottom through a diffusion mechanism, the method avoids the use of a large number of lamps, can adapt to the requirement of light intensity difference required by each stage of polymerization reaction kinetics, better meets the kinetic and thermodynamic changes in the polymerization process, and has better appearance and performance than the products sold in the market.

Moreover, the utility model adopts the multi-channel micro-tube reactor, the channel of each horizontal tube reactor is narrow, the mass transfer and heat transfer capability is strong, the materials in the reactor are mixed quickly, and the reaction heat can be taken away quickly because the horizontal tube reactor is in the constant temperature box, the reaction automatic acceleration phenomenon caused by heat accumulation is avoided, and the stability and controllability of the polymerization reaction are ensured; furthermore, the multi-channel micro-tube reactor of the utility model can be provided with a plurality of horizontal tube reactors, thus being capable of being enlarged without enlarging effect.

Adopt the utility model provides a device preparation polyacrylamide nanometer microballon can shorten reaction temperature control under normal atmospheric temperature state about 1 hour, greatly reduced the energy consumption, improved production process's economic benefits, reduced the product quality risk simultaneously.

In addition, the materials keep a certain advancing speed in the horizontal tubular reactor, and when the materials flow in the reactor, a strong scouring effect can be formed on attachments on the inner wall of the pipeline, so that the acrylamide monomer is prevented from adhering to the pipe wall to form gel, the product quality is improved, and the equipment cleaning and maintenance frequency is reduced; and in the process of advancing the materials, the back mixing phenomenon is avoided, and the complete reaction of the raw materials can be promoted.

Drawings

FIG. 1 is a schematic view of an apparatus for photo-initiation preparation of polyacrylamide nano-microspheres according to the present invention; wherein, 1 is a light source, 1-1 is a light source box, 1-2 is a lower cover plate of the light source box, 2 is a dispersion prism, 2-1 is a prism box, 2-1-1 is an upper cover plate of the prism box, 2-1-2 is a lower cover plate of the prism box, 3 is a multichannel microtube reactor, 3-1 is a thermostat, 3-1-1 is a constant temperature water inlet of the thermostat, 3-1-2 is a constant temperature water outlet of the thermostat, 3-2 is a horizontal tubular reactor, 4 is a light source control box, 5 is a light source and prism height adjusting box, 5-1 bolts, 6 is a shading box, 7 is a closed box, and 8 is a base;

FIG. 2 is a schematic diagram of the operation of the apparatus provided by the present invention; wherein, 1 is a light source, 2 is a dispersion prism, 3-2 is a horizontal tubular reactor, and 3-3 is an opaque baffle plate;

FIG. 3 is a side perspective view of a multi-channel microtube reactor provided by the present invention;

FIG. 4 is a state diagram of a horizontal tube reactor covered with different color bands;

FIG. 5 is a view showing a structure of a lifting member of the apparatus used in the embodiment of the present invention; wherein, 9 is a bracket, 10 is a gear, 11 is a hook, 12 is a gear carrier, 13 is a light source/dispersion prism, 14 is a gear guide rail, and 15 is a self-locking synchronous servo motor;

FIG. 6 is a top view of a lifting member of an apparatus used in an embodiment of the present invention; wherein, 9 is a bracket, 10 is a gear, 11 is a hook, 12 is a gear rack, and 13 is a light source/dispersion prism;

FIG. 7 particle size distribution diagram of the product obtained in example 1 for each horizontal tubular reactor;

FIG. 8 particle size distribution diagram of the product obtained in example 2 for each horizontal tubular reactor;

FIG. 9 is a graph showing the particle size distribution of the product obtained in example 3 in each horizontal tubular reactor;

FIG. 10 particle size distribution plot of the product obtained in example 4 for each horizontal tubular reactor;

FIG. 11 particle size distribution plot of the product obtained in example 5 for each horizontal tubular reactor;

FIG. 12 particle size distribution plot of the product obtained in each horizontal tube reactor of example 6;

FIG. 13 particle size distribution diagram of the product obtained in example 7 for each horizontal tubular reactor;

FIG. 14 is a graph showing the particle size distribution of the product obtained in example 8 in each horizontal tubular reactor;

FIG. 15 particle size distribution of the product obtained in example 9 for each horizontal tubular reactor;

FIG. 16 is a particle size distribution diagram of comparative example 1;

FIG. 17 particle size distribution plot for comparative example 2;

fig. 18 is a particle size distribution diagram of comparative example 3.

Detailed Description

The utility model provides a device for photoinitiation preparation polyacrylamide nanometer microballon, as shown in figure 1, including light source 1, dispersion prism 2 and multichannel microtube reactor 3, multichannel microtube reactor includes thermostated container 3-1, a plurality of horizontal tubular reactor 3-2 and a plurality of opaque baffle (not shown in figure 1), opaque baffle and horizontal tubular reactor are at the interval arrangement in the thermostated container, and opaque baffle separates each horizontal tubular reactor, the material of horizontal tubular reactor is transparent material; the light dispersion surface of the dispersion prism is positioned above the multichannel micro-tube reactor.

The working principle of the device provided by the utility model is as shown in figure 2, the horizontal tubular reactor 3-2 and the opaque baffle 3-3 are arranged at intervals, the horizontal tubular reactor and the opaque baffle are immersed in the thermostatic waterbath of the thermostat, the side perspective view of the multichannel micro-tube reactor is shown in figure 3, and the two sides of the horizontal tubular reactor are the opaque baffles. The following introduces the principle of the utility model in combination with fig. 2, the light source passes through the dispersion prism and produces different typefaces, different typefaces cover the horizontal tubular reactor in the multichannel microtube reactor respectively, form the state that each horizontal tubular reactor is covered by different typefaces, obtain the pipeline of different colours (as shown in fig. 4), after the raw materials mixed liquid is carried to horizontal tubular reactor, under different chromatic light shines, take place the photoinitiation polymerization to obtain the polyacrylamide nanometer microballon of different particle diameters at the discharge gate of horizontal tubular reactor.

The device for preparing the polyacrylamide nano microspheres by photoinitiation provided by the utility model comprises a light source, wherein the light source is preferably an incandescent lamp or an L ED lamp, the shape of the light source is not specially limited, and the produced color band can cover a multi-channel micro reactor.

In the utility model, the light source is preferably arranged in a light source box 1-1, and the light source box is preferably provided with a light source box lower cover plate 1-2; at least one side of the light box is preferably a switchable side, or at least one side of the light box is preferably provided with a switchable window. In the utility model, the light source box can protect the light source, avoid the pollution of dust to the light source, and simultaneously avoid the light generated by the light source from irradiating the outside of the device to generate light pollution; the light source box is provided with a light source box lower cover plate, so that a light source can be sealed when the light source box is not used, and the light source can be better protected; but light source box's switch side or the setting of switch window is favorable to the maintenance of equipment and observes inside.

The device for preparing polyacrylamide nano microspheres by photoinitiation provided by the utility model preferably also comprises a light source control box 4; the light source control box is used for controlling the on-off of the light source and the intensity of the light source. The utility model discloses it is right the position of light source control box does not have special restriction, and technical personnel in the field can set up as required the embodiment of the utility model provides an in, light source control box is located one side of light source box, passes through bolted connection with the light source box, and the bolt does not indicate in the picture.

The device for preparing polyacrylamide nano microspheres by photoinitiation provided by the utility model comprises a dispersion prism; the dispersion prism is preferably a dispersion prism or a dispersion tetraprism, and the refractive index of the dispersion prism is preferably 1.210-1.580.

In the utility model, the dispersion prism is preferably arranged in a prism box 2-1, and the prism box 2-1 is preferably provided with a prism box upper cover plate 2-1-1 and a prism box lower cover plate 2-1-2; at least one side of prism case is for can switching side, perhaps at least one side of prism case is provided with but switch window. In the utility model, the prism box protects the dispersion prism, so as to avoid dust pollution, and is provided with the prism box upper cover plate and the prism box lower cover plate, so that the dispersion prism can be sealed in the prism box when not in use, thereby achieving better protection effect on the dispersion prism; the openable side of the prism box or the openable window is arranged to be beneficial to the maintenance of equipment and the observation of the conditions in the box.

The device for preparing polyacrylamide nano microspheres by photoinitiation provided by the utility model preferably also comprises a light source and a prism height adjusting box 5; the light source and prism height adjusting box is used for adjusting the heights of the light source and the dispersion prism so as to obtain a proper color band. The utility model has no special limit to the position of the light source and the prism height adjusting box, and the light source and the prism height adjusting box can be arranged by the technicians in the field according to the requirement; the light source and prism height adjustment box are preferably connected to the light source control box by bolts 5-1 (as shown in fig. 1).

The utility model discloses it is right the mode that light source and prism altitude mixture control case adjusted light source and dispersion prism does not have special restriction, adopt the conventional mode that sets up in this field can. In the embodiment of the utility model, the device still includes liftable parts, light source and dispersion prism are preferred to be set up respectively on liftable parts's support, liftable parts is fixed a side of light source case or prism case, and with light source and prism altitude mixture control case communication connection.

The utility model discloses to the liftable part does not have special restriction, as long as do not shelter from light, can make the typewriter ribbon that dispersion prism produced cover horizontal tubular reactor can, in the embodiment of the utility model, the liftable part is gear formula lifting unit (as shown in fig. 5, wherein, 9 is the support, 10 is the gear, 11 is the couple, 12 is the gear frame, 13 is light source/dispersion prism, 14 is the gear guide, 15 is auto-lock synchronous servo motor), including gear, gear frame, gear guide, auto-lock synchronous servo motor and support, auto-lock synchronous servo motor uses with the gear cooperation for control gear goes up and down; the gear guide rail is attached to the inner side of the gear rack; the bracket is fixed on the gear rack, so that the gear rack drives the bracket to move up and down in the up-and-down moving process; the support and the gear rack form a certain angle, so that the support extends into the light source box or the prism box (as shown in fig. 6, the top view of the lifting component is shown, wherein 9 is the support, 10 is the gear, 11 is the hook, 12 is the gear rack, and 13 is the light source/dispersion prism), the support is provided with the hook, the light source or the dispersion prism can be hung, and the size and the length of the hook can be adjusted to adjust the angles of the light source and the dispersion prism.

In the utility model, a shading box 6 is preferably arranged between the light source box and the prism box; the shading box can avoid light source pollution, a partition plate with a hollow shape can be further arranged in the shading box to adjust the shape of light irradiated by a light source, so that the light is only irradiated on an incident surface of the dispersion prism, in addition, a certain neutral position is kept between the light source box and the prism box due to the arrangement of the shading box, and during equipment maintenance, manual operation is simple. The utility model discloses in, shading case does not have upper and lower apron, opens light source box lower cover plate and prism case upper cover plate, and light source box and prism case can be for the connected state.

The device for preparing polyacrylamide nano microspheres by photoinitiation provided by the utility model comprises a multi-channel micro-tube reactor, wherein the multi-channel micro-tube reactor comprises a constant temperature box, a plurality of horizontal tube reactors and a plurality of opaque clapboards, the opaque clapboards and the horizontal tube reactors are arranged at intervals in the constant temperature box, the opaque clapboards separate each horizontal tube reactor (as shown in figure 2), and the horizontal tube reactors are made of transparent materials; the light dispersion surface of the dispersion prism is positioned above the multichannel micro-tube reactor.

In the utility model, a closed box 7 is arranged above the multichannel microtube reactor, the prism box is positioned above the closed box, at least one side surface of the closed box is preferably a switchable side surface, or at least one side surface is preferably provided with a switchable window; the closed box can avoid light pollution; the closed box is not provided with an upper cover plate and a lower cover plate, and the prism box and the constant temperature box can be in a communicated state after the lower cover plate of the prism box and the upper cover plate of the constant temperature box are opened; the switchable side or the switchable window on the closed box is beneficial to observing the condition of the multi-channel micro-tube reactor.

In the present invention, the thermostat is preferably a constant temperature water bath. As shown in figure 1, a constant temperature water inlet 3-1-1 and a constant temperature water outlet 3-1-2 are arranged on the constant temperature water bath tank; the constant temperature water bath box is provided with a constant temperature water bath box upper cover plate 3-1-3; the upper cover plate of the constant-temperature water bath box can protect the horizontal tubular reactor and the water bath in the water bath box from being polluted when the equipment is not used.

The utility model discloses in, can set up the number of horizontal tubular reactor according to the number of used typewriter ribbon, if only when using two monochromatic typewriters, the number that sets up horizontal tubular reactor is 2. In the embodiment of the present invention, the number of the horizontal tubular reactors is preferably 7.

In the present invention, the number of the opaque partition plates is preferably one less than the number of the horizontal tubular reactors to ensure that each horizontal tubular reactor can be partitioned.

In the present invention, the transparent material is preferably quartz glass. In the present invention, the quartz glass has a good light transmittance, and light generated by dispersion is filled in a single channel (i.e., a horizontal tube reactor) from strong to weak through a diffusion mechanism from top to bottom.

The utility model discloses in, the internal diameter of horizontal tubular reactor is preferred 20 ~ 38mm, and total length is preferred 20 ~ 80m, horizontal tubular reactor's horizontal length is preferred 50 ~ 80cm, the length of dispersion prism's light dispersion surface is preferred 100 ~ 300 mm. In the utility model, the horizontal tubular reactor with the inner diameter and the length has better mass transfer and heat transfer performance, and can complete the polymerization reaction at the fastest reaction rate at the limit reaction temperature, thereby reducing the reaction time; the light dispersion surface with the length can ensure that the generated color band completely covers the multi-channel micro-tube reactor.

In the present invention, the vertical distance between the dispersion prism and the multichannel micro-tube reactor is preferably 60 to 100 cm. The utility model discloses in, above-mentioned distance is convenient for adjust the angle of dispersion prism, and the enough typewriter ribbon that makes the chromatic dispersion produce of above-mentioned distance covers the multichannel microtube reactor completely.

The utility model discloses in, the feed inlet of horizontal tubular reactor is preferred to pass through the pipeline intercommunication with the raw materials mixing kettle, the preferred material pump that is provided with on the pipeline. The utility model discloses in, the raw materials mixing kettle can be with raw materials misce bene, can realize carrying the raw material mixture to the multichannel micro-tube reactor continuously through the material pump to realize continuous production. In the utility model, the technicians in the field can adjust the number of the raw material mixing kettles according to the needs, that is, when the polyacrylamide nano microspheres with different particle diameters are needed to be prepared, the same raw material mixture can be introduced into each horizontal tubular reactor, at the moment, only one raw material mixing kettle is arranged, the pipelines with the same number as that of the horizontal tubular reactors are arranged, and the advection pumps are arranged on the pipelines; when the raw material mixture entering each horizontal tubular reactor is different, a plurality of raw material mixing kettles can be arranged for mixing different raw materials and respectively conveying the raw materials to each horizontal tubular reactor.

In the present invention, the discharge port of the horizontal tube reactor is preferably connected to a product collector.

The device for preparing polyacrylamide nano microspheres by photoinitiation provided by the utility model preferably further comprises a base 8.

The utility model also provides a preparation method of polyacrylamide nanometer microballon adopts above-mentioned technical scheme the device preparation polyacrylamide nanometer microballon specifically includes following step:

filling a constant temperature box with water, and adjusting the temperature to the temperature required by the polymerization reaction;

irradiating a visible light beam generated by a light source on a dispersion prism, wherein color bands generated by the dispersion prism respectively cover each horizontal tubular reactor;

mixing acrylamide, a surfactant, a cross-linking agent, a photoinitiator and water, continuously conveying the mixture to a horizontal tubular reactor, and collecting a product at a discharge port of the horizontal tubular reactor.

The utility model discloses at first fill the thermostated container with water, adjust to the required temperature of polymerization.

The utility model discloses in, the temperature preferred of thermostated container is 15 ~ 30 ℃.

After adjusting to the required temperature of polymerization, the utility model discloses shine visible light beam on dispersion prism, each horizontal tubular reactor is covered respectively to the typewriter ribbon that dispersion prism produced.

The utility model discloses in, the illumination intensity of visible light beam is preferred 500 ~ 5000lx, more preferred 1000 ~ 4000lx, most preferred 2000 ~ 3000 lx. In the utility model, the illumination intensity can ensure that the product meets the requirements and has no implosion phenomenon; when the illumination intensity is too high, the decomposition rate of the photoinitiator is increased, the polymerization reaction speed can be increased rapidly, the reaction heat can not be removed rapidly, and finally local overheating is caused, the polyacrylamide is in a gel form, namely 'implosion' occurs, when the illumination intensity is too low, the decomposition rate of the photoinitiator is too slow, the acrylamide is not completely involved in the reaction, the particle size of the generated polyacrylamide microsphere is small, the solid content is low, and the actual use requirement can not be met.

After the typewriter ribbon that produces when dispersion prism covers each horizontal tubular reactor respectively, the utility model discloses mix acrylamide, surfactant active, cross-linking agent, photoinitiator and water after, carry to horizontal tubular reactor in succession, collect the product at horizontal tubular reactor's discharge gate.

The utility model discloses it is right the mixing order of acrylamide, surfactant active, cross-linking agent, photoinitiator and water does not have special restriction, can obtain the mixed liquid of misce bene can, in the embodiment of the utility model, preferably mix acrylamide and water, obtain acrylamide aqueous solution, mix with surfactant active, cross-linking agent and photoinitiator again.

In the present invention, the initiator preferably includes a ferrocene photoinitiator, a silver halide photoinitiator (also referred to as a haloyellow silver photoinitiator), a biphenyl formyl photoinitiator or an organic phosphorous oxide photoinitiator; the ferrocene photoinitiator is preferably bis 2, 6-difluoro-3-pyrrolyl phenyl ferrocene; the silver halide photoinitiator is preferably silver bromide or silver iodide; the biphenyl formyl photoinitiator is preferably biphenyl formyl; the organic phosphorus oxide photoinitiator is preferably 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide. In the utility model, one or more photoinitiators can be selected and used by the technicians in the field according to the requirements, the dosage of the photoinitiators can be adjusted according to the requirements, when one photoinitiator is used and the raw material mixtures entering each horizontal tubular reactor are the same, the materials entering each horizontal tubular reactor are the same, the raw material mixtures can be directly prepared in a raw material mixing kettle and then conveyed to each horizontal tubular reactor; when one photoinitiator is used but the material ratio of the raw material mixture entering each horizontal tubular reactor is different, or a plurality of photoinitiators are used and the raw material mixture entering each horizontal tubular reactor is different, the raw materials are mixed in different raw material mixing kettles respectively to obtain different raw material mixtures, and then the raw material mixtures are conveyed to different horizontal tubular reactors respectively.

In the present invention, the crosslinking agent is preferably N, N-m-phenylene bismaleimide.

In the present invention, the molar ratio of the acrylamide to the crosslinking agent is preferably 1:0.05 to 0.2, and more preferably 1:0.01 to 0.15.

In the present invention, the mass of the photoinitiator preferably accounts for 0.01 to 0.1%, and more preferably 0.03 to 0.07% of the total mass of the acrylamide and the crosslinking agent.

In the utility model discloses, the surfactant preferably is the mixture of sorbitan fatty acid ester (span80) and polyoxyethylene sorbitan monolaurate (tween60), the mass ratio of sorbitan fatty acid ester (span80) and polyoxyethylene sorbitan monolaurate (tween60) is preferably 1: 1.0-1.5, more preferably 1: 1.2-1.3; the dosage of the surfactant is preferably 35-55% of the total mass of the raw materials (namely the sum of the mass of the acrylamide, the surfactant, the cross-linking agent and the photoinitiator).

In the utility model discloses in, the velocity of flow of carrying to the material in the horizontal tubular reactor is preferably 300 ~ 800m L/min, and more preferably 400 ~ 700m L/min.

The following embodiments are provided to describe in detail an apparatus for preparing polyacrylamide nanospheres by photoinitiation and a method for preparing polyacrylamide nanospheres, but they should not be construed as limiting the scope of the present invention.

Example 1

Preparing polyacrylamide nano microspheres by adopting the device shown in FIG. 1, wherein the light source is an incandescent lamp light source with the intensity of 500lx, the refractive index of a dispersion prism is 1.210, the length of a light dispersion surface is 160mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 90cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 30mm, the total length is 40m, the horizontal length is 75cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, and the water bath temperature in a constant temperature box is 15 ℃; a product collector is arranged at the discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a ferrocene photoinitiator (bis 2, 6-difluoro-3-pyrrole phenyl ferrocene) in a raw material mixing kettle according to the following proportion: the mol ratio of the acrylamide to the cross-linking agent is 1:0.05, and the weight of the ferrocene photoinitiator is 0.01 percent of the total mass of the acrylamide and the cross-linking agent; the mass of the surfactant accounts for 50% of the total mass of the raw materials.

And respectively conveying the mixed raw material liquid to each horizontal tubular reactor, wherein the flow velocity of the feed liquid in each horizontal tubular reactor is 300m L/min, the retention time of the feed liquid in each horizontal tubular reactor is 94.2min, and collecting the product of each horizontal tubular reactor in a product collector.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 7, where a-g are horizontal tubular reactors corresponding to a red color band, an orange color band, a yellow color band, a green color band, a cyan color band, a blue color band, and a violet color band in this order. The average particle diameters of the products obtained from the horizontal tubular reactor corresponding to the red color band to the horizontal tubular reactor corresponding to the purple color band are 57nm, 64nm, 77nm, 83nm, 97nm, 106nm and 113nm in sequence, the viscosities are 378mPa & s, 389mPa & s, 363mPa & s, 407mPa & s, 419mPa & s, 465mPa & s and 442mPa & s in sequence. After all the products are mixed, testing the solid content (namely the whole effective solid content) of the obtained mixed product, namely filtering the mixed product, drying the obtained filter cake, weighing, and dividing the mass of the dried filter cake by the mass of the mixed product to obtain the whole effective solid content of 25.62 percent; the overall conversion, i.e. the mass of product divided by the mass of starting material, was calculated to be 97.30%.

Example 2

Preparing polyacrylamide nano microspheres by adopting the device shown in FIG. 1, wherein the light source is an incandescent lamp light source with the intensity of 1000lx, the refractive index of a dispersion prism is 1.370, the length of a light dispersion surface is 100mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 60cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 32mm, the total length is 50m, the horizontal length is 80cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, and the water bath temperature in a constant temperature box is 18 ℃; a product collector is arranged at the discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and silver bromide in a raw material mixing kettle according to the following ratio: the molar ratio of the acrylamide to the cross-linking agent is 1:0.01, and the weight of the silver bromide is 0.04 percent of the total mass of the acrylamide and the cross-linking agent; the mass of the surfactant accounts for 46% of the total mass of the raw materials.

And respectively conveying the mixed raw material liquid to each horizontal tubular reactor, wherein the flow velocity of the feed liquid in each horizontal tubular reactor is 700m L/min, the retention time of the feed liquid in each horizontal tubular reactor is 57.4min, and collecting the product of each horizontal tubular reactor in a product collector.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 8, where a-g are horizontal tubular reactors corresponding to a red color band, an orange color band, a yellow color band, a green color band, a cyan color band, a blue color band, and a violet color band in this order. The average particle diameter of the product obtained from the horizontal tubular reactor corresponding to the red color band to the horizontal tubular reactor corresponding to the purple color band is 58nm, 64nm, 79nm, 85nm, 92nm, 102nm and 114nm in sequence, and the viscosity is 362mPa & s, 377mPa & s, 379mPa & s, 391mPa & s, 407mPa & s, 427mPa & s and 445mPa & s in sequence; after all the products were mixed, the resulting mixed product was tested for solids content (i.e., overall effective solids content), and the overall conversion was calculated to be 24.97% overall effective solids content and 99.11% overall reaction conversion.

Example 3

The device shown in FIG. 1 is adopted to prepare polyacrylamide nano microspheres, wherein the used light source is L ED light source with the intensity of 1500lx, the refractive index of a dispersion prism is 1.410, the length of a light dispersion surface is 120mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 100cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 24mm, the total length is 80m, the horizontal length is 60cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, the water bath temperature in a thermostat is 25 ℃, and a product collector is arranged at a discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a dibenzoyl photoinitiator (dibenzoyl) in a raw material mixing kettle according to the following ratio: the mol ratio of the acrylamide to the cross-linking agent is 1:0.12, the weight of the biphenyl formyl photoinitiator is 0.1 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 55 percent of the total mass of the raw materials;

and respectively conveying the mixed raw material liquid to each horizontal tubular reactor, wherein the flow velocity of the feed liquid in each horizontal tubular reactor is 600m L/min, the retention time of the feed liquid in each horizontal tubular reactor is 60.3min, and collecting the product of each horizontal tubular reactor in a product collector.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 9, where a-g are horizontal tubular reactors corresponding to a red color band, an orange color band, a yellow color band, a green color band, a cyan color band, a blue color band, and a violet color band in this order. The average particle size of products obtained from the horizontal tubular reactor corresponding to the red color band to the horizontal tubular reactor corresponding to the purple color band is 56nm, 64nm, 79nm, 83nm, 93nm, 106nm and 110nm in sequence, the viscosity is 356mPa & s, 361mPa & s, 383mPa & s, 389mPa & s, 404mPa & s, 417mPa & s and 425mPa & s respectively, after all the products are mixed, the solid content (namely the whole effective solid content) of the obtained mixed product is tested, the whole conversion rate is calculated, the whole effective solid content is 25.26%, and the whole reaction conversion rate is 98.73%.

Example 4

Preparing polyacrylamide nano microspheres by adopting the device shown in FIG. 1, wherein the light source is an incandescent lamp light source with the intensity of 2000lx, the refractive index of a dispersion tetraprism is 1.580, the length of a light dispersion surface is 100mm, the vertical distance between the dispersion tetraprism and a multichannel microtube reactor is 60cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 38mm, the total length is 20m, the horizontal length is 65cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion triple prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, and the water bath temperature in a thermostat is 30 ℃; a product collector is arranged at the discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and silver iodide in a raw material mixing kettle according to the following ratio: the molar ratio of the acrylamide to the cross-linking agent is 1:0.16, the weight of the silver iodide is 0.08 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 40 percent of the total mass of the raw materials;

and respectively conveying the mixed raw material liquid to each horizontal tubular reactor, wherein the flow velocity of the feed liquid in each horizontal tubular reactor is 600m L/min, the retention time of the feed liquid in each horizontal tubular reactor is 37.8min, and collecting the product of each horizontal tubular reactor in a product collector.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 10, where a to g are horizontal tubular reactors corresponding to a red color band, an orange color band, a yellow color band, a green color band, a cyan color band, a blue color band, and a violet color band in this order. The average particle size of the products obtained from the horizontal tubular reactor corresponding to the red color band to the horizontal tubular reactor corresponding to the purple color band is 55nm, 62nm, 72nm, 85nm, 96nm, 108nm and 119nm in sequence, the viscosity is 349mPa & s, 351mPa & s, 363mPa & s, 382mPa & s, 399mPa & s, 411mPa & s and 432mPa & s in sequence, after all the products are mixed, the solid content of the obtained mixed product is tested (namely the whole effective solid content), the whole effective solid content is calculated, the whole effective solid content is 24.6%, and the whole reaction conversion rate is 97.64%.

Example 5

The device shown in FIG. 1 is adopted to prepare polyacrylamide nano microspheres, wherein the used light source is L ED light source with the intensity of 750lx, the refractive index of a dispersion prism is 1.500, the length of a light dispersion surface is 300mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 90cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 28mm, the total length is 60m, the horizontal length is 70cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, the water bath temperature in a thermostat is 28 ℃, and a product collector is arranged at a discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a crosslinking agent (N, N-m-phenylene bismaleimide) and an organic phosphorus oxide photoinitiator (2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide) in a raw material mixing kettle according to the following proportion: the mol ratio of the acrylamide to the cross-linking agent is 1:0.2, the weight of the organic phosphorus oxide photoinitiator is 0.1 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 38 percent of the total mass of the raw materials;

and respectively conveying the mixed raw material liquid to each horizontal tubular reactor, wherein the flow speed of the feed liquid in each horizontal tubular reactor is 800m L/min, the retention time of the feed liquid in each horizontal tubular reactor is 46.2min, and collecting the product of each horizontal tubular reactor in a product collector.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 11, where a to g are horizontal tubular reactors corresponding to a red color band, an orange color band, a yellow color band, a green color band, a cyan color band, a blue color band, and a violet color band in this order. The average particle diameters of the products obtained from the horizontal tubular reactor corresponding to the red color band to the horizontal tubular reactor corresponding to the purple color band are 57nm, 62nm, 75nm, 86nm, 94nm, 103nm and 111nm in sequence, the viscosities are 352mPa · s, 354mPa · s, 370mPa · s, 379mPa · s, 389mPa · s, 406mPa · s and 428mPa · s in sequence, after all the products are mixed, the solid content of the obtained mixed product (namely the whole effective solid content) is tested, and the whole conversion rate is calculated, wherein the whole effective solid content is 22.91% and the whole reaction conversion rate is 95.21%.

Example 6

The device shown in FIG. 1 is adopted to prepare polyacrylamide nano microspheres, wherein a light source is an L ED lamp with the intensity of 3000lx, the refractive index of a dispersion prism is 1.260, the length of a light dispersion surface is 160mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 80cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 20mm, the total length is 50m, the horizontal length is 60cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, the water bath temperature in a thermostat is 21 ℃, and a product collector is arranged at a discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a crosslinking agent (N, N-m-phenylene bismaleimide) and an organic phosphorus oxide photoinitiator (2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide) in a raw material mixing kettle according to the following proportion: the mol ratio of the acrylamide to the cross-linking agent is 1:0.16, the weight of the organic phosphorus oxide photoinitiator is 0.03 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 40 percent of the total mass of the raw materials;

and respectively conveying the mixed raw material liquid to each horizontal tubular reactor, wherein the flow velocity of the feed liquid in each horizontal tubular reactor is 500m L/min, the retention time of the feed liquid in each horizontal tubular reactor is 31.4min, and collecting the product of each horizontal tubular reactor in a product collector.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 12, where a to g are horizontal tubular reactors corresponding to a red color band, an orange color band, a yellow color band, a green color band, a cyan color band, a blue color band, and a violet color band in this order. The average particle diameters of products obtained from the horizontal tubular reactor corresponding to the red color band to the horizontal tubular reactor corresponding to the purple color band are 55nm, 61nm, 76nm, 83nm, 94nm, 108nm and 113nm in sequence, the viscosities are 359mPa & s, 350mPa & s, 367mPa & s, 391mPa & s, 407mPa & s and 428mPa & s in sequence, after all the products are mixed, the solid content of the obtained mixed product (namely the whole effective solid content) is tested, the whole effective solid content is calculated, the whole effective solid content is 23.8%, and the whole reaction conversion rate is 99.24%.

Example 7

The polyacrylamide nanospheres are prepared by adopting the device shown in FIG. 1, wherein a light source is an L ED lamp with the intensity of 5000lx, the refractive index of a dispersion prism is 1.290, the length of a light dispersion surface is 220mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 75cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 30mm, the total length is 60m, the horizontal length is 50cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, the water bath temperature in a thermostat is 21 ℃, and a product collector is arranged at a discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a ferrocene photoinitiator (bis 2, 6-difluoro-3-pyrrole phenyl ferrocene) in a raw material mixing kettle according to the following proportion to obtain a raw material mixed solution containing the ferrocene photoinitiator: the mol ratio of the acrylamide to the cross-linking agent is 1:0.2, the weight of the ferrocene photoinitiator is 0.05 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 44 percent of the total mass of the raw materials;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a biphenyl formyl photoinitiator (biphenyl formyl) in a raw material mixing kettle according to the following ratio to obtain a raw material mixed solution containing the biphenyl formyl photoinitiator: the mol ratio of the acrylamide to the cross-linking agent is 1:0.2, the weight of the biphenyl formyl photoinitiator is 0.02 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 35 percent of the total mass of the raw materials;

conveying the raw material mixed solution containing the ferrocene photoinitiator to a horizontal tubular reactor covered by a red color band, wherein the flow speed of the feed liquid is 700m L/min, and the retention time of the feed liquid in the horizontal tubular reactor is 60.6 min;

conveying the raw material mixed liquid containing the biphenyl formyl photoinitiator to a horizontal tubular reactor covered by a purple color band, wherein the flow rate of the material liquid is 800m L/min, and the retention time of the material liquid in the horizontal tubular reactor is 53.0 min;

the product of each horizontal tubular reactor was collected in a product collector.

The product from each collector was dispersed in white oil and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE nanosizer from Malvern Panalytical corporation, the results of which are shown in FIG. 13, where a and b are horizontal tubular reactors corresponding to the red and purple bands in this order. The average particle size of the product obtained by the horizontal tubular reactor corresponding to the red color band is 54nm, the viscosity is 347mPa & s, the average particle size of the product obtained by the horizontal tubular reactor corresponding to the purple color band is 55nm, the viscosity is 353mPa & s, the overall effective solid content is 23.48%, and the overall reaction conversion rate is 99.03%.

Example 8

The polyacrylamide nanospheres are prepared by adopting the device shown in FIG. 1, wherein a light source is an L ED lamp with the intensity of 3000lx, the refractive index of a dispersion prism is 1.436, the length of a light dispersion surface is 240mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 85cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 32mm, the total length is 40m, the horizontal length is 50cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, the water bath temperature in a thermostat is 18 ℃, and a product collector is arranged at a discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a biphenyl formyl photoinitiator (biphenyl formyl) in a raw material mixing kettle according to the following ratio to obtain a raw material mixed solution containing the biphenyl formyl photoinitiator: the mol ratio of the acrylamide to the cross-linking agent is 1:0.15, the weight of the biphenyl formyl photoinitiator is 0.1 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 41 percent of the total mass of the raw materials;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and an organic phosphorus oxide photoinitiator (2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide) in a raw material mixing kettle according to the following proportion to obtain a raw material mixed solution containing the organic phosphorus oxide photoinitiator: the mol ratio of the acrylamide to the cross-linking agent is 1:0.15, the weight of the organic phosphorus oxide photoinitiator is 0.04 percent of the total mass of the acrylamide and the cross-linking agent, and the mass of the surfactant accounts for 47 percent of the total mass of the raw materials;

conveying the raw material mixed liquid containing the biphenyl formyl photoinitiator to a horizontal tubular reactor covered by a blue color band, wherein the flow rate of the feed liquid is 600m L/min, and the retention time of the feed liquid in the horizontal tubular reactor is 53.6 min;

conveying a raw material mixed solution containing an organic phosphorus oxide photoinitiator to a horizontal tubular reactor covered by a purple color band, wherein the flow rate of the feed liquid is 800m L/min, and the retention time of the feed liquid in the horizontal tubular reactor is 40.2 min;

The products from each collector were separately dispersed in white oil and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE nanosizer from Malvern Panalytical corporation, the results of which are shown in FIG. 14, where a and b are horizontal tubular reactors corresponding to blue and violet bands in this order. The average particle size of the product obtained by the horizontal tubular reactor corresponding to the blue color band is 111nm, the viscosity is 436 mPa.s, the average particle size of the product obtained by the horizontal tubular reactor corresponding to the purple color band is 119nm, the viscosity is 448 mPa.s, the overall effective solid content is 23.77%, and the overall reaction conversion rate is 96.73%.

Example 9

The device shown in FIG. 1 is adopted to prepare polyacrylamide nano microspheres, wherein a light source is an L ED lamp with the intensity of 3000lx, the refractive index of a dispersion prism is 1.478, the length of a light dispersion surface is 240mm, the vertical distance between the dispersion prism and a multichannel microtube reactor is 70cm, the multichannel microtube reactor comprises 7 horizontal tubular reactors, the inner diameter of each horizontal tubular reactor is 32mm, the total length is 30m, the horizontal length is 70cm, an opaque partition plate is arranged between the horizontal tubular reactors, the positions of the light source and the dispersion prism are adjusted, seven color bands generated by dispersion are respectively covered on the 7 horizontal tubular reactors, the water bath temperature in a thermostat is 14 ℃, and a product collector is arranged at a discharge port of each horizontal tubular reactor;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a biphenyl formyl photoinitiator (biphenyl formyl) in a raw material mixing kettle according to the following ratio to obtain a raw material mixed solution A, wherein the molar ratio of acrylamide to the cross-linking agent is 1:0.15, the weight of the biphenyl formyl photoinitiator is 0.1 percent of the total mass of the acrylamide and the cross-linking agent, the mass of the surfactant accounts for 50 percent of the total mass of the raw material, conveying the raw material mixed solution A to a horizontal tubular reactor covered by a yellow color band, the flow rate of the raw material liquid is 500m L/min, and the retention time of the raw material liquid in the horizontal tubular reactor is 48.2 min;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a biphenyl formyl photoinitiator (biphenyl formyl) in a raw material mixing kettle according to the following ratio to obtain a raw material mixed solution B, wherein the molar ratio of acrylamide to the cross-linking agent is 1:0.15, the weight of the biphenyl formyl photoinitiator is 0.08 percent of the total mass of the acrylamide and the cross-linking agent, the mass of the surfactant accounts for 45 percent of the total mass of the raw material, conveying the raw material mixed solution B to a horizontal tubular reactor covered by a green color band, the flow rate of the material liquid is 600m L/min, and the retention time of the material liquid in the horizontal tubular reactor is 40.2 min;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60 which are mixed according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a biphenyl formyl photoinitiator (biphenyl formyl) in a raw material mixing kettle according to the following ratio to obtain a raw material mixed solution C, wherein the molar ratio of acrylamide to the cross-linking agent is 1:0.15, the weight of the biphenyl formyl photoinitiator is 0.04 percent of the total mass of the acrylamide and the cross-linking agent, the mass of the surfactant accounts for 32 percent of the total mass of the raw material, conveying the raw material mixed solution C to a horizontal tubular reactor covered by a blue color band, the flow rate of the material liquid is 700m L/min, and the retention time of the material liquid in the horizontal tubular reactor is 34.5 min;

mixing an acrylamide aqueous solution, a surfactant (namely span80 and tween60) in a raw material mixing kettle according to the mass ratio of 1: 1.2), a cross-linking agent (N, N-m-phenylene bismaleimide) and a biphenyl formyl photoinitiator (biphenyl formyl) in a raw material mixing kettle according to the following ratio to obtain a raw material mixed solution D, wherein the molar ratio of acrylamide to the cross-linking agent is 1:0.15, the weight of the biphenyl formyl photoinitiator is 0.03 percent of the total mass of the acrylamide and the cross-linking agent, the mass of the surfactant accounts for 45 percent of the total mass of the raw material, conveying the raw material mixed solution D to a horizontal tubular reactor covered by a purple color band, the flow rate of the raw material liquid is 800m L/min, and the retention time of the raw material liquid in the horizontal tubular reactor is 30.1 min.

The products in each collector were dispersed in white oil, and the average particle size and particle size distribution were measured using a Zetasizer Nano ZSE Nano-particle sizer from Malvern Panalytical, the results of which are shown in fig. 15, where a to d are horizontal tubular reactors corresponding to yellow, green, blue and violet bands in order. The average particle size of the product obtained by the horizontal tubular reactor corresponding to the yellow color band is 111nm, the viscosity is 409 mPa.s, the average particle size of the product obtained by the horizontal tubular reactor corresponding to the green color band is 113nm, the viscosity is 413 mPa.s, the average particle size of the product obtained by the horizontal tubular reactor corresponding to the blue color band is 114nm, the viscosity is 431 mPa.s, the average particle size of the product obtained by the horizontal tubular reactor corresponding to the purple color band is 119nm, the viscosity is 428 mPa.s, the overall effective solid content is 24.42%, and the overall reaction conversion rate is 98.90%.

Comparative example 1

Polyacrylamide emulsion product with the brand of BSA-508, produced by Beijing stone Daodel technologies, Inc.

The solid content is 20.74 percent and the viscosity is 1011 mPas through tests, which shows that the solid content meets the specification of SY/T5862 and 2008 polymer technical requirements for oil displacement in the China oil and gas industry standard, but the product has higher viscosity and higher requirement on the pressure bearing capacity of a pump and a matched pipeline during use.

The particle size distribution of this comparative example was measured by the method of example 1, and as a result, a flat peak appeared as shown in fig. 16, and the particle size distribution was wide and the distribution range was poor in uniformity.

Comparative example 2

A polyacrylamide emulsion product manufactured by Shandong Nuo Er Biotechnology Co., Ltd under the trade name SNE-024.

The solid content is 21.62 percent and the viscosity is 857 mPa.s through tests, which shows that the solid content meets the specification of SY/T5862 and 2008 polymer technical requirements for oil displacement in the China oil and gas industry standard, but the product has higher viscosity and higher requirements on a pump and a matched pipeline during use.

The particle size distribution of this comparative example was measured by the method of example 1, and as a result, a flat peak appeared as shown in fig. 17, and the particle size distribution was wide and the distribution range was poor in uniformity.

Comparative example 3

A polyacrylamide emulsion product with the brand number of RX-615 is produced by New petrochemical company Limited in Shanxi.

The solid content is 21.13 percent and the viscosity is 1244mPa & s through tests, which shows that the solid content meets the specification of SY/T5862-.

The particle size distribution of this comparative example was measured by the method of example 1, and as a result, as shown in fig. 18, a double peak appeared, and the particle size distribution was wide and the distribution range was poor in uniformity.

The light transmission of the product obtained by the horizontal tubular reactor corresponding to the blue color band in example 2, the product obtained by the horizontal tubular reactor corresponding to the yellow color band in example 4, and the products obtained by comparative examples 2 and 3 is tested, and the test result shows that the product obtained by the method provided by the utility model has more excellent light transmission and can show the gap between background papers, while the light transmission of the products obtained by comparative examples 2 and 3 is poor and can not show the gap between background papers.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims

1. The device for preparing the polyacrylamide nano-microspheres by photoinitiation is characterized by comprising a light source, a dispersion prism and a multi-channel micro-tube reactor, wherein the multi-channel micro-tube reactor comprises a constant temperature box, a plurality of opaque partition plates and a plurality of horizontal tube reactors, the opaque partition plates and the horizontal tube reactors are arranged at intervals in the constant temperature box, the opaque partition plates separate the horizontal tube reactors, and the horizontal tube reactors are made of transparent materials; the light dispersion surface of the dispersion prism is positioned above the multichannel micro-tube reactor.

2. The apparatus of claim 1, wherein the apparatus for photoinitiating preparation of the polyacrylamide nanospheres further comprises a light source control box for controlling on/off of the light source and intensity of the light source.

3. The apparatus of claim 1 or 2, wherein the apparatus for photoinitiating preparation of polyacrylamide nanospheres further comprises a light source and a prism height adjusting box for adjusting the height of the light source and the dispersion prism.

4. The apparatus of claim 3, wherein the light source is disposed in a light source box, the dispersing prism is disposed in a prism box, and a light shielding box is disposed between the light source box and the prism box.

5. The apparatus of claim 4, wherein a closed box is disposed above the multichannel microtube reactor, and the prism box is located above the closed box.

6. The apparatus according to claim 1 or 4, wherein the dispersion prism is a dispersion triple prism or a dispersion quadruple prism, and the refractive index of the dispersion prism is 1.210-1.580.

7. The apparatus of claim 1, wherein the horizontal tubular reactor has an inner diameter of 20 to 38mm, a total length of 20 to 80m, and a horizontal length of 50 to 80 cm; the length of the light dispersion surface of the dispersion prism is 100-300 mm.

8. The apparatus of claim 1, wherein the incubator is a constant temperature water bath.

9. The device according to any one of claims 1 to 2,4 to 5 and 7 to 8, wherein a feed inlet of the horizontal tube type reactor is communicated with the raw material mixing kettle through a pipeline, and a material pump is arranged on the pipeline.

10. The apparatus according to any one of claims 1 to 2 and 4 to 8, wherein the discharge port of the horizontal tube reactor is provided with a product collector.