CN111592624B - Method for preparing general comprehensive polycarboxylate superplasticizer - Google Patents
Method for preparing general comprehensive polycarboxylate superplasticizer Download PDFInfo
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- CN111592624B CN111592624B CN201910165749.4A CN201910165749A CN111592624B CN 111592624 B CN111592624 B CN 111592624B CN 201910165749 A CN201910165749 A CN 201910165749A CN 111592624 B CN111592624 B CN 111592624B
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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Abstract
The invention discloses a method and a device for preparing a general comprehensive polycarboxylic acid water reducing agent. The method adopts a multi-component copolymerization method to synthesize the general comprehensive polycarboxylic acid water reducing agent, and raw materials comprise unsaturated polyether macromonomer, unsaturated carboxylic acid small monomer, anti-mud functional monomer, starch and modified starch monomer thereof, tap water purifying agent, slump-retaining functional monomer, retardation functional monomer, preservative, initiator, chain transfer agent, oxidant, reducing agent and alkali liquor; the device of the invention is of a distributed annular matrix structure. The method of the invention has strong operability, and the prepared water reducing agent has good comprehensive performance and working performance; the device has strong operability and can improve the working efficiency; the prepared product has the advantages of uniform components, stable quality, novel structure, small occupied area, low processing cost, easy industrial production, potential industrial value and application prospect.
Description
Technical Field
The invention relates to the field of concrete water reducing agent preparation, in particular to a method and a device for preparing a general comprehensive polycarboxylic acid water reducing agent.
Background
The polycarboxylate superplasticizer is a new generation high-efficiency superplasticizer, and is divided into a slow-setting type, a slow-release type, an early-strength type, a slump retaining type, a mud-resistant and salt-resistant type, a general comprehensive type and the like according to the performances and application occasions of the polycarboxylate superplasticizer. Unfortunately, most researches are still conducted in a laboratory shake flask bench stage, and a high-efficiency industrial production method and a process device for synthesizing the general comprehensive polycarboxylate superplasticizer by adopting a multi-polymerization method are not developed at present.
The preparation method of the polycarboxylate superplasticizer generally relates to a chemical solid-liquid reaction system, and correspondingly comprises a solid-phase and liquid-phase feeding device, a reaction kettle reaction device, a heating device and the like. When the conventional polycarboxylic acid water reducing agent is prepared, a liquid-phase reaction material has good fluidity, and the liquid-phase reaction material is easily added into a reaction kettle by a flowmeter and a pipeline for conveying and feeding; solid-phase reactant feeding, particularly powder feeding, is difficult to feed into a reaction vessel due to poor flowability of powder, and is usually slowly and manually fed into a reactor after being weighed by metering or fed into the reactor by a belt conveyor or a vacuum feeding device.
And to the reation kettle of polycarboxylate water reducing agent preparation industrialization device or production system design in-process, adopt "I" type, "L" type, "H" type or "U" mode design and installation a plurality of reation kettle usually, the reaction head tank can only erect reinforced directly over reation kettle, wherein the blowing of reaction solid material jar can only be transported to in a reation kettle through a band conveyer, a band conveyer can not be reinforced several reation kettle, the difficult problem of reaction powder feeding appears. Therefore, the addition of the powder to a plurality of reaction vessels requires a plurality of reaction raw material tanks in cooperation with a plurality of belt conveyors, which complicates the charging system.
Meanwhile, the water reducing agent obtained by the reaction is put into a storage tank, and the water reducing agent in the storage tank is deposited for a period of time to influence the performance of the water reducing agent.
In order to solve the problems, scientific research workers and production technicians must develop an industrial production method and device for efficiently preparing the general comprehensive polycarboxylate superplasticizer by adopting multi-polymerization, and a storage device which is convenient for the efficient and accurate feeding, the efficient reaction and the precipitation prevention of various solid-liquid materials of multi-polymerization, and can almost meet the requirements of various general comprehensive polycarboxylate superplasticizer production systems. However, no relevant report of a universal and efficient comprehensive polycarboxylic acid water reducer industrial production method and process device for multi-polymerization preparation is available at present.
Disclosure of Invention
One purpose of the invention is to provide a method for preparing a general comprehensive polycarboxylic acid water reducing agent; the invention also aims to provide a device for preparing the general comprehensive polycarboxylic acid water reducing agent.
The device of the invention perfects the defects that the addition of various reaction materials of the general comprehensive polycarboxylate superplasticizer preparation process device is not easy to control, the reaction efficiency is not high, and the product is easy to generate precipitate and cannot be back-mixed to eliminate the precipitate. The method adopts a weighing and reacting solid-phase ingredient of a weighing bin and a feeding mode of a liquid-blending tank group matched with a precision flowmeter to measure a reacting liquid-phase ingredient, can accurately control the adding amount of solid-phase and liquid-phase reacting materials, adopts a mode of adding the reacting solid-phase ingredient into a reaction device by adopting a zigzag steering lifting conveying device, adopts a mode of adding the reacting liquid-phase ingredient into the reaction device by adopting a mode of adding the liquid-blending tank group matched with an annular liquid discharge pipe in a circumferential distribution manner, adopts a mode of adopting an annular matrix distributed reaction kettle group, adopts an annular matrix distributed storage tank group matched with an annular circulating pipe in a circumferential distribution manner, adds the materials into a reaction kettle in an internal and external circulation manner, effectively solves most problems in the production method and process device for preparing the general comprehensive polycarboxylate superplasticizer by adopting a multi-polymerization method at present, greatly improves the operability of a reaction production system for preparing the general comprehensive polycarboxylate superplasticizer, Universality, improved working efficiency, product component uniformity and quality stability
In order to achieve the purpose, the method for preparing the general comprehensive polycarboxylate superplasticizer adopts multicomponent copolymerization to synthesize the general comprehensive polycarboxylate superplasticizer, and the synthesis raw materials comprise: by mass fraction, 100 parts of unsaturated polyether macromonomer A, 20-60 parts of unsaturated carboxylic acid small monomer B, 10-20 parts of anti-mud functional monomer C, 5-20 parts of starch and modified starch monomer D, 80-100 parts of tap water purifying agent E, 10-20 parts of slump-retaining functional monomer F, 10-20 parts of retardation functional monomer G, 0.05 part of preservative H, 0.5-3 parts of initiator I, 0.5-0.8 part of chain transfer agent J, 0.3-3 parts of oxidant K, 0.1-0.5 part of reducing agent L and alkali liquor M, wherein the amount of the alkali liquor M is used for adjusting the pH of the mixed raw material to be 6-7;
the unsaturated polyether macromonomer A comprises one or more of allyl alcohol polyoxyethylene ether (APEG, the number average molecular weight is 1500-2400), polyethylene glycol monomethyl ether (MPEG, the number average molecular weight is 1500-2400), methyl allyl polyoxyethylene ether (TPEG, the number average molecular weight is 1500-2400), and prenol polyoxyethylene ether (HPEG, the number average molecular weight is 1500-2400);
the unsaturated carboxylic acid small monomer B comprises one or more of acrylic acid, methacrylic acid, sodium propylene sulfonate, maleic acid, maleic anhydride and itaconic acid;
the anti-mud type functional monomer C comprises one or more of low-price acrylamide, sodium silicate, sodium metasilicate pentahydrate, sodium tripolyphosphate, polyvinyl alcohol, polyethylene glycol, ethylenediamine, disodium ethylene diamine tetraacetate, sodium humate, sodium polyacrylate, sodium styrene sulfonate and beta-cyclodextrin;
the starch and modified starch monomer D thereof comprises one or more of common corn starch, wheat starch, potato starch, gelatinized starch and sulfonated starch;
the tap water purifying agent E is hexamethylenetetramine, and the added amount of the hexamethylenetetramine is as follows: 250g of hexamethylenetetramine/1000 Kg of water;
the slump-retaining functional monomer F comprises one or more of styrene, hydroxyethyl acrylate, ethyl p-hydroxybenzoate, N dimethylene phosphoric acid amino maleate, dimethylaminoethyl methacrylate, sulfonated cellulose and sulfonated lignin;
the retarding functional monomer G comprises one or more of glucose, sodium gluconate, white sugar, sodium citrate, tartaric acid, sodium tartrate, sodium hexametaphosphate, sodium pyrophosphate, sodium pentaglycolate and boric acid;
the preservative H is dimethyl fumarate;
the initiator I comprises a composite initiator such as ammonium persulfate/sodium bisulfite, ammonium persulfate/hydrogen peroxide, potassium permanganate/oxalic acid, hydrogen peroxide/ascorbic acid and the like;
the chain transfer agent J comprises one or more of thioglycolic acid, mercaptoethanol and sodium methacrylate sulfonate;
the oxidant K comprises one or more of hydrogen peroxide, ammonium persulfate, potassium ammonium persulfate, ammonium sodium persulfate and potassium permanganate;
the reducing agent L comprises one or more of vitamin C, ferrous sulfate, sodium bisulfite, sodium metabisulfite and sodium hypophosphite;
the alkali liquor M comprises one of sodium hydroxide and potassium hydroxide with the mass concentration of 40%.
The method for preparing the general comprehensive polycarboxylate superplasticizer adopts multicomponent copolymerization to synthesize the general comprehensive polycarboxylate superplasticizer, and comprises the following implementation steps of: the raw materials comprise the following components in percentage by mass:
1) adding 100 parts of unsaturated polyether macromonomer A, 5-20 parts of starch and modified starch monomer D5 into a reaction device of a reaction kettle group, adding tap water purifying agent E80-100 parts, stirring, mixing and dissolving, then sequentially adding 20-60 parts of unsaturated carboxylic acid small monomer B, 0.3-3 parts of oxidant K, 75-20 parts of slump-retaining functional monomer F10, 0.1-0.5 part of reducing agent L, 0.5-3 parts of initiator I and 0.5-0.8 part of chain transfer agent J, naturally cooling to 30 ℃ after the reaction is completed, adding alkali liquor M, adjusting the pH value to 6-7, adding 0.05 part of preservative H, and aging to obtain the general comprehensive polycarboxylic acid water reducer product with the solid content of about 40%.
The device for preparing the general comprehensive polycarboxylate superplasticizer comprises an equipment support, wherein a liquid-phase batching storage tank group and a solid-phase batching storage tank are arranged above the equipment support, and a metering bin weighing device, a zigzag steering lifting conveying device, a reaction kettle group, a 1# heating device, a finished product storage tank group, a mixing and stirring kettle and a 2# heating device are arranged below the equipment support; a zigzag steering lifting conveying device is arranged below the weighing device of the metering bin, the zigzag steering lifting conveying device is connected with a reaction kettle group, and the reaction kettle group is distributed in a central annular matrix by using the zigzag steering lifting conveying device; the reaction kettle group is respectively connected with a 1# heating device and a finished product storage tank group, and the finished product storage tank group is sequentially connected with a mixing stirring kettle and a 2# heating device.
The liquid phase batching storage tank group comprises eight liquid phase batching storage tank groups distributed in an annular matrix, wherein the eight liquid phase batching storage tank groups comprise a 1# liquid phase batching storage tank, a 2# liquid phase batching storage tank, a 3# liquid phase batching storage tank, a 4# liquid phase batching storage tank, a 5# liquid phase batching storage tank, a 6# liquid phase batching storage tank, a 7# liquid phase batching storage tank and an 8# liquid phase batching storage tank; a stirring shaft is arranged in the No. 1 liquid phase batching storage tank, a stirring motor is installed at one end of the stirring shaft, stirring blades are arranged on the stirring shaft, a liquid level meter scale is arranged on a tank body of the No. 1 liquid phase batching storage tank, a communicated liquid level meter is arranged on a tank body of the liquid phase batching storage tank group, a liquid inlet is arranged at the top of each liquid phase batching storage tank group, liquid outlets are arranged at the bottoms of the liquid phase batching storage tank groups, the liquid outlets are all connected with a pipeline and a flow meter, a liquid discharge control pipe valve is installed between the pipeline and the flow meter, and the other end of the pipeline is arranged in the reaction kettle group; the solid-phase batching storage tank mainly comprises a solid-phase batching storage tank cavity, wherein a feed inlet is formed in the top of the solid-phase batching storage tank cavity, a discharge pipe orifice is formed in the bottom of the solid-phase batching storage tank cavity, and a star-shaped discharger is arranged on the discharge pipe orifice.
The weighing device of the measuring bin comprises a solid material discharge inlet pipe connected to the measuring bin through a connecting hose, a platform balance/platform scale is arranged under the measuring bin, a platform balance/platform scale supporting platform is arranged under the platform balance/platform scale, two ends of the platform balance/platform scale supporting platform are mounted on a hanger fixing plate through two platform balance/platform scale supporting platform fixing hangers vertically arranged left and right, and a star-shaped discharger is arranged at the lower end of the weighing device of the measuring bin.
The zigzag-shaped turning, lifting and conveying device consists of a zigzag-shaped material lifting and conveying belt and a turning mechanism; the zigzag material lifting conveying belt comprises a conveying belt and a conveying belt carrier roller support matched with the conveying belt, and the conveying belt is provided with an upper end parallel section, a middle inclined section and a lower end parallel section; a conveying belt supporting roller is arranged below the conveying belt; the conveying belt carrier roller is connected with a speed reducing motor through a motor transmission belt; a conveying belt vertical supporting rod is arranged below the conveying belt carrier roller support and is arranged on the steering mechanism;
the steering mechanism comprises an annular track and a supporting connecting rod arranged in the center of the annular track;
the conveying belt vertical supporting rod is clamped by a conveying belt vertical supporting rod left clamping plate and a conveying belt vertical supporting rod right clamping plate and then is arranged on an annular track of the steering mechanism;
a rolling bearing is arranged between the left clamping plate of the vertical support rod of the conveying belt and the right clamping plate of the vertical support rod of the conveying belt; the corresponding positions of the left clamp plate of the vertical support rod of the conveying belt and the right clamp plate of the vertical support rod of the conveying belt are provided with shaft holes, the shaft holes correspond to the shaft holes on the rolling bearing, and a rotating shaft penetrates through the shaft holes of the left clamp plate of the vertical support rod of the conveying belt and the right clamp plate of the vertical support rod of the conveying belt and the shaft holes on the rolling bearing;
the annular track is provided with a positioning hole; the positioning hole is matched with the positioning bolt;
the upper end part of the support connecting rod is welded with the lower part of the conveying belt carrier roller bracket, and the lower end part of the support connecting rod penetrates through and is fixed on the rolling bearing;
the rolling bearing seat is arranged in the bearing sleeve, and the bearing sleeve flanging is provided with a bearing sleeve hinge part; the bearing sleeve support is arranged at the bottom of the bearing sleeve, and the bearing sleeve support is flanged and provided with a bearing sleeve support hinge part; the bearing sleeve and the bearing sleeve support are fastened by a pre-buried countersunk head screw and a nut through a bearing sleeve hinge part and a bearing sleeve support hinge part;
the bearing bush support is fixed in a cement foundation in a grouting mode, and the upper end face of the bearing bush support is 5mm higher than the ground;
the rotation angle of the steering mechanism is 360 degrees horizontally.
Eight reaction kettles are distributed in the annular matrix of the reaction kettle group, an annular liquid inlet main pipe of the reaction kettle group is arranged above the reaction kettle group and surrounds the eight reaction kettles, a connecting pipe valve and a liquid inlet branch pipe of the reaction kettle group are arranged on the annular liquid inlet main pipe of the reaction kettle group, the connecting pipe valve is connected with a tank body of the liquid phase batching storage tank group, reaction kettle liquid phase batching liquid inlets are respectively arranged on the tops of the eight reaction kettles, and the liquid inlet branch pipe of the reaction kettle group is connected with the liquid phase batching liquid inlet of the reaction kettles; the bottoms of the eight reaction kettles are respectively provided with a reaction kettle group liquid discharge branch pipe valve, a reaction kettle group annular liquid discharge main pipe is arranged below the reaction kettle group and around the eight reaction kettles, and the reaction kettle group liquid discharge branch pipe valve is connected with the reaction kettle group annular liquid discharge main pipe; a liquid discharge pump liquid inlet pipe valve is connected to the annular liquid discharge main pipe of the reaction kettle group, the liquid discharge pump liquid inlet pipe valve is sequentially connected with a liquid discharge pump of the reaction kettle group and a liquid discharge pump liquid outlet pipe valve, a coil type heating pipe is arranged on the reaction kettle, one end of the coil type heating pipe is connected with a water return pipe valve of the coil type heating pipe, the other end of the coil type heating pipe is connected with a water inlet pipe valve of the coil type heating pipe, and a stirrer controlled by a stirring motor is arranged in the reaction kettle; the eight reaction kettles comprise a No. 1 reaction kettle, a No. 2 reaction kettle, a No. 3 reaction kettle, a No. 4 reaction kettle, a No. 5 reaction kettle, a No. 6 reaction kettle, a No. 7 reaction kettle and a No. 8 reaction kettle; the eight reaction kettles are sequentially communicated through a high-level communicating pipe valve of the reaction kettle group; a liquid outlet pipe valve of the liquid discharge pump is connected with the finished product storage tank group; a No. 1 heating device is arranged between the water return pipe valve of the coiled heating pipe and the water inlet pipe valve of the coiled heating pipe.
The No. 1 heating device comprises a heating water tank, a heating water tank backwater inlet is arranged at the upper end of the heating water tank, and the heating water tank backwater inlet is sequentially connected with a heating water tank backwater pipe valve and an annular backwater main pipe; a heating water tank water outlet pipe is arranged at the lower end of the heating water tank and is sequentially connected with a heating water tank water outlet control valve, a No. 1 hot water pump, a hot water pump water outlet pipe valve and an annular water inlet main pipe; the top end of the heating water tank is provided with a raw water inlet, a manhole and a thermometer, the bottom of the heating water tank is provided with a sewage discharge outlet, and an electric heater is installed in the heating water tank.
The finished product storage tank group consists of a transport pipe fitting and four finished product storage tanks, the transport pipe fitting comprises a finished product storage tank group annular liquid inlet main pipe, one end of the finished product storage tank group annular liquid inlet main pipe is provided with a finished product storage tank group liquid inlet main pipe control valve, and the other end of the finished product storage tank group annular liquid inlet main pipe is provided with a finished product storage tank group circulating liquid inlet main pipe control valve; the finished product storage tank group circulation liquid inlet branch pipe and the finished product storage tank group circulation liquid inlet branch pipe are connected to the finished product storage tank group annular liquid inlet main pipe, and a finished product storage tank group circulation liquid inlet main pipe control pipe valve is respectively connected with a finished product storage tank group discharge pipe valve and a circulation liquid discharge pump discharge pipe valve; the top of the finished product storage tank is provided with a finished product storage tank group circulation liquid inlet and a finished product storage tank group liquid inlet, the finished product storage tank group circulation liquid inlet is connected with the finished product storage tank group circulation liquid inlet through a branch pipe, and the finished product storage tank group liquid inlet is connected with the finished product storage tank group liquid inlet through a branch pipe;
the four finished product storage tanks comprise a 1# finished product storage tank, a 2# finished product storage tank, a 3# finished product storage tank and a 4# finished product storage tank; the four finished product storage tanks are communicated with each other through a finished product storage tank group high-level communicating pipe valve at the upper part of the finished product storage tank and a finished product storage tank group low-level communicating pipe valve at the lower part of the finished product storage tank in sequence; a finished product storage tank discharge port is formed in the bottom of the finished product storage tank, and a finished product storage tank discharge port pipe valve is arranged on the finished product storage tank discharge port; a finished product storage tank group annular liquid drainage main pipe is arranged around the bottoms of the four finished product storage tanks;
the discharge hole pipe valve of the finished product storage tank is connected with the annular liquid discharge main pipe of the finished product storage tank group;
a liquid inlet control pipe valve of a circulating liquid discharge pump is arranged on the annular liquid discharge main pipe of the finished product storage tank group and is connected with the circulating liquid discharge pump; and a liquid level gauge graduated scale and a communication type liquid level gauge are arranged on the finished product storage tank.
The mixing and stirring kettle comprises a mixing and stirring kettle chamber and a pipe fitting for connecting the finished product storage tank group and the No. 2 heating device, wherein the pipe fitting comprises a mixing and stirring kettle liquid discharge pump discharge control pipe valve arranged at the top of the mixing and stirring kettle chamber, and a liquid discharge control pipe valve and a mixing and stirring kettle liquid discharge pump arranged at the bottom of the mixing and stirring kettle chamber; a heating pipe is wound outside the mixing and stirring kettle, one end of the heating pipe is connected with a coil pipe type heating pipe water return pipe valve, and the other end of the heating pipe is sequentially connected with a coil pipe type heating pipe water inlet pipe valve, a No. 2 hot water pump and a heating water tank water outlet control pipe valve; and a heating water tank is arranged between the coil pipe type heating pipe water return pipe valve and the heating water tank water outlet control pipe valve.
The invention discloses a method and a device for preparing a general comprehensive polycarboxylate superplasticizer, which have the following beneficial effects:
(1) for the preparation method of the general comprehensive polycarboxylic acid water reducer, the general comprehensive polycarboxylic acid water reducer is synthesized by adopting a multi-copolymerization method according to the combination of various raw materials with different performances and low price and easy obtaining, and the method is favorable for playing the role of each functional group, so that the balance and adjustment among the performances of water reduction, dispersion, slump retaining, mud resistance and the like of the water reducer are realized;
(2) for a general comprehensive polycarboxylate superplasticizer production device, a suspension type metering bin weighing device and a solid-phase ingredient metering and feeding device matched with a zigzag steering lifting conveying device are adopted to accurately weigh, control and steer lift and convey solid-phase ingredients respectively, and the solid-phase ingredients are added into a reaction kettle group which is formed by a plurality of reaction kettles and has an annular matrix distributed structure; the precise flow control and the stepwise addition of the liquid-phase ingredients into the reaction kettle group are respectively realized by adopting a liquid-phase ingredient metering and feeding device which is matched with the liquid-phase ingredient storage tank group and the annular liquid inlet main pipe; for the heating device of the reaction kettle group, an annular water inlet main pipe and an annular water return main pipe which are arranged at the periphery of the reaction kettle group are matched with the coil type heating pipes of the reaction kettles, and the heating control of the reaction kettles is respectively realized; for the product storage and anti-precipitation circulation device of the finished product storage tank group, the annular matrix distributed finished product storage tank group, a heatable mixing and stirring kettle for preventing product precipitation, and an annular liquid inlet main pipe (annular circulation liquid inlet main pipe) and an annular liquid outlet main pipe of the finished product storage tank group are matched to respectively control the product storage, anti-precipitation circulation and discharge;
(3) by the preparation method and the process device, the operability of a production system for producing the general comprehensive polycarboxylic acid water reducing agent by multi-polymerization is greatly improved, and the working efficiency, the uniformity of product components and the stability of quality are improved; meanwhile, the whole production system and the equipment device have the characteristics of novel structure, simplicity, continuity, convenience in operation, small occupied area, low processing cost and easiness in industrialization, and have potential industrialization value and application prospect.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a front view of the assembly of the position between the liquid ingredient storage tank set 2 and the solid ingredient storage tank 3 according to the present invention;
FIG. 3 is a top view of FIG. 2;
FIG. 4 is a schematic view of the assembly of the components of the present invention;
FIG. 5 is a plan view showing the assembly of the parts of the present invention
FIG. 6 is a schematic structural view of a zigzag-shaped turning, lifting and conveying device 5 of the present invention;
FIG. 7 is an enlarged partial view A of FIG. 6;
FIG. 8 is a schematic structural view of the circular track 525 of FIG. 6;
FIG. 9 is an enlarged partial view B of FIG. 6;
in the drawings, 1-equipment rack; 2-liquid phase batching storage tank group; 201-1# liquid phase ingredient storage tank; 201-1-stirring motor; 201-2-liquid inlet; 201-3-stirring shaft; 201-4-stirring blade; 201-5-a level gauge scale; 201-6-communicating type level gauge; 201-7-liquid outlet; 201-8-drainage control tube valve; 202-2# liquid phase ingredient storage tank; 203-3# liquid phase ingredient storage tank; 204-4# liquid phase batching storage tank; 205-5# liquid phase ingredient storage tank; 206-6# liquid phase ingredient storage tank; 207-7# liquid phase batching storage tank; 208-8# liquid phase batching storage tank;
3-solid phase ingredient storage tank; 301-solid phase ingredient storage tank cavity; 302-a feed inlet; 303-star discharger; 304-a discharge nozzle;
4-a weighing device of the measuring bin; 401-hanger plate; 402-platform scale/platform scale support platform fixed hanger; 403-a metering bin; 404-connecting a hose; 405-discharging the solid material into a pipe; 406-scale/platform balance; 407-scale/platform scale support platform; 408-a star discharger;
a 5- 'zigzag' steering lifting conveying device; a 51- "zigzag" shaped material lifting conveyer belt; 511-conveyer belt idler; 512-motor drive belt; 513-a conveyor belt; 514-conveyor idler supports; 515-a reduction motor; 516-conveyor belt vertical support bar; 517A-the left splint of the vertical support rod of the conveyer belt; 517B-right splint for vertical support rod of conveyer belt; 52-a steering device; 521-a support link; 522-rolling bearing; 523-bearing sleeve; 524-bearing bush support; 525-a circular track; 525-1-positioning holes; 525-2-positioning bolts; 526-bearing housing hinge section; 527-bearing housing mount hinge section; 528-pre-burying a countersunk head screw and a nut; 529-cement foundation;
6-reaction kettle group; 601-connecting a pipe valve; 602-a reaction kettle group annular liquid inlet main pipe; 603-5# reaction kettle; 6031-solid material inlet of reaction kettle; 6032-stirring motor; 6033-branch liquid inlet pipe of the reaction kettle group; 6034-liquid inlet of reaction kettle liquid phase material; 6035-stirrer; 604-positive displacement pump discharge pipe valve; no. 605-1 reaction kettle; 6051-liquid discharge tube dividing valve of reaction kettle group; 6052-coiled pipe heating pipe water inlet pipe valve; 6053-coiled pipe type heating pipe return water pipe valve; 6054-coiled heating tube; 606-a reaction kettle group annular liquid discharge main pipe; 607-drain pump of reaction kettle group; 608-liquid discharge pump liquid inlet pipe valve;
7-1# heating device; 701-heating a water tank; 702-a sewage draining outlet; 703-an electric heater; 704-a thermometer; 705-raw water inlet; 706-manhole; 707-heating water tank backwater inlet; 708-heating water tank return pipe valve; 709-a ring-shaped water return main pipe; 710-ring-shaped water inlet main; 711-hot water pump outlet pipe valve; 712-1# hot water pump; 713-heating tank water outlet control valve; 714-heating water tank outlet pipe;
8-finished product storage tank group; 801-a finished product storage tank group liquid inlet main pipe control valve; 802-finished product storage tank group circulating liquid inlet branch pipe; 803-finished product storage tank group liquid inlet branch pipe; 804-finished product storage tank group high-level communicating pipe valve; 805-finished product storage tank group annular liquid inlet main pipe; 806-a finished product storage tank group circulating liquid inlet main pipe control pipe valve; 807-finished product storage tank group discharge pipe valve; 808-circulation drain pump discharge pipe valve; 809-a finished product storage tank group annular liquid discharge main pipe; 810-circulation drain pump; 811-3# finished product storage tank; 812-a finished product storage tank group low-level communicating pipe valve; 813-1# finished product storage tank; 8131-finished product storage tank group circulation liquid inlet; 8132-finished product storage tank group liquid inlet; 8133-level gauge scale; 8134-a communicating type level gauge; 8135-discharge opening of finished product storage tank; 8136-product tank discharge gate pipe valve; 816-circulating liquid discharge pump liquid inlet control pipe valve;
9-mixing and stirring the mixture in a kettle; 901-a mixing and stirring kettle chamber; 902-drain control tube valve; 903-mixing stirring kettle liquid discharge pump; 904-discharge control pipe valve of liquid discharge pump of mixing and stirring kettle;
10-2# heating device; 1001-heating water tank; 1002-a coil pipe type heating pipe water return pipe valve; 1003-heating water tank water outlet control pipe valve; 1004-2# hot water pump; 1005-coil pipe type heating pipe water inlet pipe valve.
Detailed Description
Example 1
The invention relates to a method for preparing a general comprehensive polycarboxylate superplasticizer, which adopts multicomponent copolymerization to synthesize the general comprehensive polycarboxylate superplasticizer and comprises the following steps:
(1) preparing raw materials:
preparation of unsaturated polyether macromonomer a: weighing 800Kg (by 50 parts) of allyl alcohol polyoxyethylene ether APEG, 1500 number average molecular weight and 800Kg (by 50 parts) of polyethylene glycol monomethyl ether MPEG, the number average molecular weight is 1500, and waiting for standby;
preparation of starch and modified starch monomer D: weighing 5 parts of common corn starch, 5 parts of gelatinized starch and 5 parts of sulfonated starch for later use;
preparation of preservative F: weighing 0.05 part of dimethyl fumarate, and placing in a beaker for later use;
the liquid preparation in the 1-8 # batching storage tank in the liquid-phase batching storage tank group 2 is as follows:
preparation of tap water: the liquid preparation in the No. 1 ingredient storage tank is as follows: adding a plurality of tap water (250g of hexamethylenetetramine/1000 Kg of water) added with the tap water purifying agent E into a No. 1 batching storage tank of the liquid-phase batching storage tank group 2 for later use;
preparing an unsaturated carboxylic acid small monomer B solution: adding 20 parts of acrylic acid, 10 parts of sodium propylene sulfonate, 10 parts of maleic acid and 50 parts of tap water into a No. 2 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a solution B for later use;
preparing an oxidant K solution: adding 0.8 part of ammonium persulfate and 15 parts of tap water into a No. 3 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a solution I for later use;
preparing a mixed solution of a reducing agent L and a chain transfer agent J: adding 0.1 part of vitamin C, 0.2 part of sodium bisulfite, 0.5 part of thioglycolic acid, 0.2 part of sodium methacrylate and 30 parts of tap water into a No. 4 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for dissolving to obtain a mixed solution of L and J for later use;
preparing an initiator I solution: adding 1.5 parts of hydrogen peroxide/ascorbic acid (the mass ratio is 3: 1) and 15 parts of tap water into a No. 5 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for dissolving to obtain a solution I for later use;
preparing a mixed solution of a retarding functional monomer G and an anti-mud functional monomer C: adding 5 parts of white sugar, 5 parts of glucose, 10 parts of sodium hexametaphosphate, 5 parts of acrylamide, 2.5 parts of sodium metasilicate pentahydrate, 2.5 parts of sodium tripolyphosphate, 2.5 parts of sodium humate, 2.5 parts of polyethylene glycol 800, 2.5 parts of ethylenediamine, 2.5 parts of beta-cyclodextrin and 40 parts of tap water into a No. 6 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a mixed solution of G and C for later use;
preparing a slump-retaining functional monomer F solution: adding 5 parts of styrene, 5 parts of hydroxyethyl acrylate, 5 parts of N, N dimethylene phosphoric acid amino maleic acid ester, 5 parts of sodium lignin sulfonate and 20 parts of tap water into a No. 7 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a solution F for later use;
preparing an alkali liquor M solution: adding sodium hydroxide with the alkali liquor of 40% in mass concentration into the No. 8 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for later use;
(2) metering and adding solid-phase ingredients:
firstly, 800Kg of allyl alcohol polyoxyethylene ether APEG with the number average molecular weight of 1500 is put into a solid phase batching storage tank 3, the materials are weighed and discharged by a weighing device 4 of a metering bin, and a zigzag steering lifting conveying device 5 is used for steering lifting conveying, and 100Kg of APEG materials are added into 1# to 8# reaction kettles in a reaction kettle group 6 with an annular matrix distributed structure; adding 800Kg of polyethylene glycol monomethyl ether MPEG, the number average molecular weight of 1500 and the average MPEG amount of 100Kg into 1# to 8# reaction kettles in a reaction kettle group 6 in an annular matrix distributed structure by using the same operation mode;
secondly, respectively weighing 8 equal parts of 10Kg of common corn starch, 10Kg of gelatinized starch and 10Kg of sulfonated starch, and respectively adding the weighed materials into No. 1-8 reaction kettles in the reaction kettle group 6;
(3) metering, adding and heating reaction of liquid-phase ingredients:
adding the prepared liquid in the 1# to 8# liquid phase batching storage tanks 201 to 208 of the liquid phase batching storage tank group 2 in a circumferential distributed structure or an annular matrix distributed structure into each reaction kettle of the reaction kettle group 6 in sequence by controlling the liquid discharge control pipe valves 201 to 8 at the lower ends of the batching storage tanks to be matched with a flow meter on a pipeline, namely adding the prepared liquid in the 1# to 8# liquid phase batching storage tanks 201 to 208 of the batching storage tank group 2 into the 1# to 8# reaction kettles of the reaction kettle group 6 according to the sequence required by production, and heating and polymerizing;
firstly, opening preheated 60 ℃ tap water in a No. 1 batching storage tank 201 of a liquid phase batching storage tank group 2, and discharging the tap water into a ring-shaped liquid inlet main pipe 602 arranged right above a reaction kettle group 6 by matching a liquid outlet pipe valve 201-8 at the lower end of the tap water with a flow meter on a pipeline, and then feeding the tap water into each 200Kg of No. 1 to No. 8 reaction kettles of the reaction kettle group 6 through a liquid inlet branch pipe 6033 on the ring-shaped liquid inlet main pipe 602, stopping material conveying, stirring and dissolving the tap water to prepare a bottom liquid with the concentration of 50 percent;
secondly, starting circulating hot water at 70-80 ℃ of the heating device 7, and heating the bodies of the reaction kettles of the reaction kettle group 6 through heat exchange of a coil heating pipe 6054;
thirdly, respectively and sequentially starting a small unsaturated carboxylic acid monomer B solution in a No. 2 batching storage tank of the liquid-phase batching storage tank group 2, an oxidant K solution in a No. 3 batching storage tank, a mixed solution of a reducing agent L and a chain transfer agent J in the No. 4 batching storage tank, an initiator I solution in the No. 5 batching storage tank, a mixed solution of a delayed coagulation type functional monomer G and an anti-mud type functional monomer C in the No. 6 batching storage tank and a slump retaining type functional monomer F solution in the No. 7 batching storage tank at a constant temperature of 65-70 ℃, controlling respective flow rates to be slowly added into a No. 1-8 reaction kettle of the reaction kettle group 6 according to a sequence, and requiring that the adding amount in the No. 1-8 reaction kettle is respectively: 180Kg of unsaturated carboxylic acid small monomer B solution, 31.6Kg of oxidant K solution, 62Kg of mixed solution of reducing agent L and chain transfer agent J, 33Kg of initiator I solution, 160Kg of mixed solution of retardation type functional monomer G and anti-mud type functional monomer C, and 80Kg of slump retaining type functional monomer F solution, wherein the dripping completion time in a 1# to 8# reaction kettle is required to be 3 hours, and an intermittent stepwise adding mode is adopted, and each material is added circularly once every 30 min. Stirring and mixing the mixture in a catalytic oxidation-reduction system to perform reactions such as multicomponent copolymerization, polycondensation and the like;
fourthly, after the feeding in the third step is finished, stopping heating, naturally cooling to 30 ℃ under slow stirring, starting a flow control system of sodium hydroxide alkali liquor M solution with the mass concentration of 40% in an 8# batching storage tank of the liquid-phase batching storage tank group 2, adding the alkali liquor M solution to 40Kg of 1# to 8# reaction kettles of the reaction kettle group 6, adjusting the pH value to 6.6, and uniformly stirring and mixing;
fifthly, respectively weighing 8 equal parts of 100g dimethyl fumarate, adding the weighed materials into a No. 1-8 reaction kettle, slowly stirring for 5min, stopping stirring, continuously aging for 1h, finishing the reaction, and discharging to obtain a general comprehensive polycarboxylic acid water reducer product with the solid content of 40% and the total weight of 6700Kg, wherein the mark is PC-T-1;
(4) storage and anti-settling cycle of the product:
the prepared products in the reaction kettle group 6 are pumped into a finished product storage tank group 8 which is formed by 1# to 4# finished product storage tanks and distributed in an annular matrix mode through an annular liquid inlet main pipe under the action of a liquid discharge pump 607 of the reaction kettle group 6, and the products are stored in a standing mode to wait for use or sale. When the finished product storage tank group 8 is placed for a period of time and precipitates appear at the lower ends of the storage tanks in the finished product storage tank group 8, a circulating liquid discharge pump arranged at the periphery of the lower end of the finished product storage tank group 8 is started, precipitate liquid at the lower parts of the storage tanks of the finished product storage tank group 8 is pumped into a mixing and stirring kettle 9 through an annular liquid discharge main pipe, a 2# heating device 10 is started to heat the product material containing the precipitates in the mixing and stirring kettle 9 through a coiled heat exchange pipe, under the stirring action of a stirring device of the mixing and stirring kettle 9, after the material liquid is heated and stirred for a period of time, the material liquid in the mixing and stirring kettle 9 is uniformly mixed, the precipitates are dissolved and disappear, and the stirring is stopped; starting a liquid discharge pump at the bottom of the mixing and stirring kettle 9, and pumping the water reducing agent after the sediment is eliminated into a corresponding storage tank of the finished product storage tank group 8 again; or when the product is used or sold, the circulating system is started to ensure that the product in the finished product storage tank group 8 is uniformly mixed through the mixing and stirring kettle 9, and then the product is pumped into the mixing and stirring kettle 9 through the finished product storage tank group 8 and discharged through the discharge pipe valve 807 of the mixing and stirring kettle 9.
Example 2
The invention relates to a method for preparing a general comprehensive polycarboxylate superplasticizer, which adopts multicomponent copolymerization to synthesize the general comprehensive polycarboxylate superplasticizer and comprises the following steps:
(1) preparing raw materials:
preparation of unsaturated polyether macromonomer A: weighing 800Kg (by 50 parts) of methyl allyl polyoxyethylene ether (TPEG, 2400) and 800Kg (by 50 parts) of prenyl polyoxyethylene ether (HPEG, 2400) for later use;
preparation of starch and modified starch monomer D: weighing 5 parts of common wheat starch, 5 parts of gelatinized starch and 5 parts of sulfonated starch for later use;
preparation of preservative F: weighing 0.05 part of dimethyl fumarate, and placing in a beaker for later use;
the liquid preparation in the 1-8 # batching storage tank in the liquid-phase batching storage tank group 2 is as follows:
preparation of tap water: the liquid preparation in the No. 1 ingredient storage tank is as follows: adding a plurality of tap water (250g of hexamethylenetetramine/1000 Kg of water) added with the tap water purifying agent E into a No. 1 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for later use;
preparing a solution of unsaturated carboxylic acid small monomer B: adding 20 parts of sodium propylene sulfonate, 10 parts of maleic acid, 10 parts of itaconic acid and 50 parts of tap water into a No. 2 ingredient storage tank of a liquid-phase ingredient storage tank group 2 for dissolving to obtain a solution B for later use;
preparing an oxidant K solution: adding 1.0 part of hydrogen peroxide and 15 parts of tap water into a No. 3 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a K solution for later use;
preparation of a mixed solution of a reducing agent L and a chain transfer agent J: adding 0.2 part of vitamin C, 0.2 part of sodium metabisulfite, 0.6 part of mercaptoethanol and 30 parts of tap water into a No. 4 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a mixed solution of L and J for later use;
preparing an initiator I solution: 2.0 parts of ammonium persulfate/hydrogen peroxide (the mass ratio is 1: 1) and 15 parts of tap water are added into a No. 5 ingredient storage tank of the liquid-phase ingredient storage tank group 2 to be dissolved, and a solution I is obtained for later use;
preparing a mixed solution of a retarding functional monomer G and an anti-mud functional monomer C: adding 5 parts of sodium citrate, 5 parts of tartaric acid, 5 parts of sodium pyrophosphate, 5 parts of sodium pentaglycolate, 2.5 parts of acrylamide, 2.5 parts of sodium silicate, 2.5 parts of polyvinyl alcohol, 2.5 parts of sodium humate, 2.5 parts of sodium styrene sulfonate, 2.5 parts of disodium ethylene diamine tetraacetate, 5 parts of beta-cyclodextrin and 40 parts of tap water into a No. 6 ingredient storage tank of a liquid-phase ingredient storage tank group 2 for dissolving to obtain a mixed solution of G and C for later use;
preparing a slump-retaining functional monomer F solution: adding 5 parts of ethyl p-hydroxybenzoate, 5 parts of dimethylamino ethyl methacrylate, 5 parts of cellulose sulfate, 5 parts of sodium lignin sulfonate and 20 parts of tap water into a No. 7 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for dissolving to obtain a solution F for later use;
preparing an alkali liquor M solution: adding sodium hydroxide with the alkali liquor of 40% in mass concentration into the No. 8 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for later use;
(2) metering and adding solid-phase ingredients:
firstly, 800Kg of methyl allyl polyoxyethylene ether (TPEG, with the number average molecular weight of 2400) is put into a solid-phase batching storage tank 3, the materials are weighed and discharged by a metering bin weighing device 4, and the reversed-Y-shaped reversed-direction lifting conveying device 5 turns to lift and convey the materials, and the TPEG materials with the average amount of 100Kg are added into 1# to 8# reaction kettles in a reaction kettle group 6 with an annular matrix distributed structure; adding 800Kg of prenyl polyoxyethylene ether (HPEG, number average molecular weight 2400), 100Kg of HPEG each into 1# -8# reaction kettle in a reaction kettle group 6 in an annular matrix distributed structure by the same operation mode;
secondly, respectively weighing 8 equal parts of 10Kg of common wheat starch, 10Kg of gelatinized starch and 10Kg of sulfonated starch, and adding the materials into a 1# to 8# reaction kettle;
(3) metering, adding and heating reaction of liquid-phase ingredients:
step one, as in example 1, prepare a 50% base solution;
secondly, the bodies of the reaction kettles of the reaction kettle group 6 were heated in the same manner as in example 1;
thirdly, at the constant temperature of 65-70 ℃, respectively and sequentially starting a solution B of the unsaturated carboxylic acid small monomer in the 2# batching storage tank of the liquid-phase batching storage tank group 2, a solution K of the oxidant in the 3# batching storage tank, a mixed solution of the reducing agent L and the chain transfer agent J in the 4# batching storage tank, a solution I of the initiator in the 5# batching storage tank, a mixed solution of the retarding functional monomer G and the anti-mud functional monomer C in the 6# batching storage tank, and a solution F of the slump-retaining functional monomer in the 7# batching storage tank, controlling respective flow rates to be slowly added into the 1# to 8# reaction kettles of the reaction kettle group 6 according to a sequence, and requiring that the adding amounts in the 1# to 8# reaction kettles are respectively: 180Kg of unsaturated carboxylic acid small monomer B solution, 32Kg of oxidant K solution, 62Kg of mixed solution of reducing agent L and chain transfer agent J, 34Kg of initiator I solution, 160Kg of mixed solution of retardation type functional monomer G and anti-mud type functional monomer C, and 80Kg of slump retaining type functional monomer F solution, wherein the dripping completion time in a 1# to 8# reaction kettle is required to be 3 hours, and an intermittent stepwise adding mode is adopted, and each material is added once in every 30min in a circulating manner. Stirring and mixing the mixture in a catalytic oxidation-reduction system to perform reactions such as multicomponent copolymerization, polycondensation and the like;
fourthly, after the feeding in the third step is finished, stopping heating, naturally cooling to 30 ℃ under slow stirring, starting a flow control system of sodium hydroxide alkali liquor M solution with the mass concentration of 40% in an 8# batching storage tank of the liquid-phase batching storage tank group 2, adding the alkali liquor M solution to 40Kg of 1# to 8# reaction kettles of the reaction kettle group 6, adjusting the pH value to 6.4, and uniformly stirring and mixing;
fifthly, respectively weighing 100g dimethyl fumarate in 8 equal parts, adding the dimethyl fumarate into a 1# to 8# reaction kettle, stirring slowly for 5min, stopping stirring, continuing aging for 1h, and discharging to obtain a general comprehensive polycarboxylic acid water reducer product with the solid content of about 40% and the total weight of about 6700Kg, wherein the general comprehensive polycarboxylic acid water reducer product is marked as PC-T-2;
(4) storage and anti-settling cycle of the product: the procedure was exactly the same as in (4) in example 1.
Example 3
(1) Preparing raw materials:
preparation of unsaturated polyether macromonomer a: weighing 400Kg (by 25 parts) of allyl alcohol polyoxyethylene ether (APEG, number average molecular weight 1500), 400Kg (by 25 parts) of polyethylene glycol monomethyl ether (MPEG, number average molecular weight 1500), 400Kg (by 25 parts) of methyl allyl polyoxyethylene ether (TPEG, number average molecular weight 1500) and 400Kg (by 25 parts) of isopentenol polyoxyethylene ether (HPEG, number average molecular weight 1500) for later use;
preparation of starch and modified starch monomer D: weighing 5 parts of common potato starch, 5 parts of gelatinized starch and 5 parts of sulfonated starch for later use;
preparation of preservative F: weighing 0.05 part of dimethyl fumarate, and placing in a beaker for later use;
the liquid preparation in the 1-8 # batching storage tank in the liquid-phase batching storage tank group 2 is as follows:
preparation of tap water: the liquid preparation in the No. 1 ingredient storage tank is as follows: adding a plurality of tap water (250g of hexamethylenetetramine/1000 Kg of water) added with the tap water purifying agent E into a No. 1 batching storage tank of the liquid-phase batching storage tank group 2 for later use;
preparing an unsaturated carboxylic acid small monomer B solution: adding 10 parts of methacrylic acid, 10 parts of sodium propylene sulfonate, 10 parts of maleic acid, 10 parts of itaconic acid and 50 parts of tap water into a No. 2 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for dissolving to obtain a solution B for later use;
preparing an oxidant K solution: adding 1.2 parts of hydrogen peroxide, 1.0 part of ammonium persulfate and 15 parts of tap water into a No. 3 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for dissolving to obtain a K solution for later use;
preparation of a mixed solution of a reducing agent L and a chain transfer agent J: adding 0.2 part of vitamin C, 0.2 part of sodium bisulfite, 0.1 part of ferrous sulfate, 0.5 part of mercaptoethanol, 0.2 part of sodium methacrylate and 30 parts of tap water into a No. 4 ingredient storage tank of a liquid-phase ingredient storage tank group 2 for dissolving to obtain a mixed solution of L and J for later use;
preparing an initiator I solution: adding 1.5 parts of ammonium persulfate/sodium bisulfite (the mass ratio is 1: 1) and 15 parts of tap water into a No. 5 ingredient storage tank of a liquid-phase ingredient storage tank group 2 for dissolving to obtain a solution I for later use;
preparing a mixed solution of a retarding functional monomer G and an anti-mud functional monomer C: adding 2.5 parts of sodium gluconate, 2.5 parts of white sugar, 2.5 parts of sodium citrate, 2.5 parts of tartaric acid, 5 parts of sodium hexametaphosphate, 5 parts of sodium pentaglycolate, 2.5 parts of acrylamide, 2.5 parts of sodium silicate, 2.5 parts of polyvinyl alcohol, 2.5 parts of sodium humate, 2.5 parts of sodium styrene sulfonate, 2.5 parts of ethylenediamine, 2.5 parts of sodium tripolyphosphate, 2.5 parts of beta-cyclodextrin and 40 parts of tap water into a No. 6 batching storage tank of the liquid-phase batching storage tank group 2 for dissolving to obtain a mixed solution of G and C for later use;
preparing a slump-retaining functional monomer F solution: adding 2.5 parts of styrene, 2.5 parts of hydroxyethyl acrylate, 2.5 parts of ethyl p-hydroxybenzoate, 2.5 parts of N, N dimethylene phosphoric acid amidomaleate, 2.5 parts of dimethylamino ethyl methacrylate, 2.5 parts of cellulose sulfate, 2.5 parts of sodium lignin sulfonate and 20 parts of tap water into a No. 7 ingredient storage tank of a liquid phase ingredient storage tank group 2 for dissolving to obtain an F solution for later use;
preparing an alkali liquor M solution: adding sodium hydroxide with the alkali liquor of 40% in mass concentration into the No. 8 ingredient storage tank of the liquid-phase ingredient storage tank group 2 for later use;
2) metering and adding solid-phase ingredients:
firstly, 400Kg of allyl alcohol polyoxyethylene ether (APEG, number average molecular weight 1500) is put into a solid phase batching storage tank 3, the materials are weighed and discharged by a metering bin weighing device 4, and a zigzag steering lifting conveying device 5 is used for steering lifting conveying, and APEG materials with the average amount of 50Kg are added into 1# to 8# reaction kettles in a reaction kettle group 6 in an annular matrix distributed structure; respectively and sequentially adding 400Kg of polyethylene glycol monomethyl ether (MPEG, the number average molecular weight is 1500), 400Kg of methyl allyl polyoxyethylene ether (TPEG, the number average molecular weight is 1500) and 400Kg of isoamyl alcohol polyoxyethylene ether (HPEG, the number average molecular weight is 1500) into No. 1 to No. 8 reaction kettles in a reaction kettle group 6 by the same operation mode, wherein the average amount of each 50Kg is respectively;
secondly, respectively weighing 8 equal parts of 10Kg of common potato starch, 10Kg of gelatinized starch and 10Kg of sulfonated starch, and adding the weighed materials into a 1# to 8# reaction kettle;
3) metering, adding and heating reaction of liquid-phase ingredients:
step one, as in example 1, prepare a 50% base solution;
secondly, heating the reaction kettle bodies of the reaction kettle group 6 in the same way as in the example 1;
thirdly, respectively and sequentially starting a small unsaturated carboxylic acid monomer B solution in a No. 2 batching storage tank of the liquid-phase batching storage tank group 2, an oxidant K solution in a No. 3 batching storage tank, a mixed solution of a reducing agent L and a chain transfer agent J in the No. 4 batching storage tank, an initiator I solution in the No. 5 batching storage tank, a mixed solution of a delayed coagulation type functional monomer G and an anti-mud type functional monomer C in the No. 6 batching storage tank and a slump retaining type functional monomer F solution in the No. 7 batching storage tank at a constant temperature of 65-70 ℃, controlling respective flow rates to be slowly added into a No. 1-8 reaction kettle of the reaction kettle group 6 according to a sequence, and requiring that the adding amount in the No. 1-8 reaction kettle is respectively: 180Kg of unsaturated carboxylic acid small monomer B solution, 34.4Kg of oxidant K solution, 62.4Kg of mixed solution of reducing agent L and chain transfer agent J, 33Kg of initiator I solution, 160Kg of mixed solution of retardation type functional monomer G and anti-mud type functional monomer C, and 75Kg of slump retaining type functional monomer F solution, wherein the completion time of dripping in a 1# to 8# reaction kettle is required to be 3 hours, and an intermittent stepwise adding mode is adopted, and each material is added circularly once every 30 min. Stirring and mixing the mixture in a catalytic oxidation-reduction system to perform reactions such as multicomponent copolymerization, polycondensation and the like;
fourthly, after the feeding in the third step is finished, stopping heating, naturally cooling to 30 ℃ under slow stirring, starting a flow control system of sodium hydroxide alkali liquor M solution with the mass concentration of 40% in an 8# batching storage tank of the liquid-phase batching storage tank group 2, adding the alkali liquor M solution to 40Kg of 1# to 8# reaction kettles of the reaction kettle group 6, adjusting the pH value to 6.1, and uniformly stirring and mixing;
fifthly, respectively weighing 8 equal parts of 100g dimethyl fumarate, adding the weighed materials into a No. 1-8 reaction kettle, slowly stirring for 5min, stopping stirring, continuously aging for 1h, finishing the reaction, and discharging to obtain a general comprehensive polycarboxylic acid water reducer product with the solid content of 40% and the total weight of 6700Kg, wherein the mark is PC-T-3;
4) storage and anti-settling cycle of the product: the procedure was exactly the same as in 4) of example 1.
And (3) performance testing:
the fluidity of the cement paste prepared from the general comprehensive polycarboxylic acid water reducing agent prepared in the embodiment 1-3 is tested, the test method refers to GB/T8077-2012, namely the homogeneity test method of concrete admixture, the used cement is P42.5R ordinary portland cement in Qilianshan of Gansu province, the W/C is 0.29, the bending and fixing mixing amount of the water reducing agent is 0.60 wt% (relative to the cement using amount), the soil substituted cement in sand and stones in northwest regions is tested by the internal mixing method to be 6.8%, and the test result of the fluidity of the cement paste is shown in Table 1.
The slump and the compressive strength of a test piece of the concrete prepared by the general comprehensive polycarboxylic acid water reducing agent prepared in the embodiment 1-3 are tested, wherein the slump test of the concrete is tested according to GB/T50080-2002 Standard of Performance test method of common concrete mixture, the compressive strength of the test piece is tested according to GB/T17671-1999 Cement Strength test method, the used cement is Gansu Kelianshan P42.5R common Portland cement, the mineral powder is wine steel S95 level mineral powder, the fly ash is second-level ash, the sand is machine-made sand and contains 6.0% of mud and medium sand with fineness modulus of 2.6, the stone with particle size of 5-25 contains 0.8% of mud, and the total mud content of the sandstone component is 6.8%; the mass ratio of the components in the concrete is 170: 90: 80: 810: 1070: 150; the bending and consolidation mixing amount of the water reducing agent is 0.60 wt% (relative to the cement amount), the water reducing agent is added according to the proportion, the stirring time is 180 seconds, the vibrating time is 15 seconds, the glue-sand ratio is 1: 3, the test is carried out under the condition that the total mud content of actual sandstone components is 6.8%, and the test result of the concrete performance is shown in Table 2.
TABLE 1 Cement paste fluidity test results (soil content: 6.8% of the mass of the substituted cement as a blending amount)
TABLE 2 slump and test piece compressive strength test results of the concrete (soil content: total soil content in actual sandstone component 6.8% as the content)
As can be seen from table 1: the cement paste prepared by the embodiment 1-3 of the general comprehensive polycarboxylate superplasticizer provided by the invention has the advantages that under the condition that the doping amount is low (0.60%) and the cement is replaced by soil is 6.8%, the initial fluidity can reach 240mm, the 60-min fluidity can reach about 210mm, the cement paste fluidity shows good fluidity, the cement paste fluidity is high, the time loss is low, the cement paste fluidity loss within 1h can be ensured to be low, and meanwhile, the cement paste has a high water reducing rate which can reach 30%.
As can be seen from table 2: the concrete prepared by the embodiments 1-3 of the universal comprehensive polycarboxylic acid water reducing agent disclosed by the invention has good slump and compressive strength of a test piece under the conditions that the mixing amount is 0.60% and the cement is 6.8% by replacing soil, the initial slump is more than 190mm, the slump after 60min is more than 180mm, the slump retaining performance is good, the slump loss of the concrete within 2h is reduced, the initial working efficiency of the concrete is better improved, and meanwhile, the water reducing rate is higher and can reach 27%.
In summary, it can be seen from tables 1 and 2 that: the embodiments 1-3 of the universal comprehensive polycarboxylic acid water reducing agent prepared by the invention are used in the prepared cement paste and concrete, have good comprehensive performance and working performance, have good dispersibility and plasticity retention under a small mixing amount (0.60%), have high water reducing rate, fast development of early strength, high later strength, obvious high strength performance and good anti-soil effect, are particularly suitable for being used in occasions with sand and stone content less than 8% in northwest, have low air content, good workability of concrete and no bleeding and segregation phenomena, and the comprehensive performance of the universal comprehensive polycarboxylic acid water reducing agent also meets the requirement of long-distance conveying in commercial concrete engineering within 60 min.
Claims (2)
1. A method for preparing a general comprehensive polycarboxylate superplasticizer is characterized by comprising the following steps: the general comprehensive polycarboxylate superplasticizer is synthesized by adopting multicomponent copolymerization, and the synthesis raw materials comprise: the modified starch-based composite material comprises, by mass, 100 parts of an unsaturated polyether macromonomer A, 20-60 parts of an unsaturated carboxylic acid small monomer B, 10-20 parts of an anti-mud functional monomer C, 5-20 parts of a starch and modified starch monomer D5, 100 parts of a tap water purifying agent E80, 10-20 parts of a slump-retaining functional monomer F10, 35-20 parts of a retardation functional monomer G10, 0.05 part of a preservative H, 0.5-3 parts of an initiator I, 0.5-0.8 part of a chain transfer agent J, 0.3-3 parts of an oxidant K, 0.1-0.5 part of a reducing agent L and an alkali liquor M, wherein the alkali liquor M is used for adjusting the pH of the mixed raw material to 6-7;
the unsaturated polyether macromonomer A comprises one or more of allyl alcohol polyoxyethylene ether, polyethylene glycol monomethyl ether, methyl allyl polyoxyethylene ether and isoamylol polyoxyethylene ether;
wherein the number average molecular weight of the allyl alcohol polyoxyethylene ether is 1500-2400;
the number average molecular weight of the polyethylene glycol monomethyl ether is 1500-2400;
the number average molecular weight of the methyl allyl polyoxyethylene ether is 1500-2400;
the number average molecular weight of the prenyl polyoxyethylene ether is 1500-2400;
the unsaturated carboxylic acid small monomer B comprises one or more of acrylic acid, methacrylic acid, sodium propylene sulfonate, maleic acid, maleic anhydride and itaconic acid;
the anti-mud type functional monomer C comprises one or more of low-price acrylamide, sodium silicate, sodium metasilicate pentahydrate, sodium tripolyphosphate, polyvinyl alcohol, polyethylene glycol, ethylenediamine, disodium ethylene diamine tetraacetate, sodium humate, sodium polyacrylate, sodium styrene sulfonate and beta-cyclodextrin;
the starch and modified starch monomer D thereof comprises one or more of common corn starch, wheat starch, potato starch, gelatinized starch and sulfonated starch;
the tap water purifying agent E is hexamethylenetetramine, and the added amount of the hexamethylenetetramine is as follows: 250g of hexamethylenetetramine/1000 Kg of water;
the slump-retaining functional monomer F comprises one or more of styrene, hydroxyethyl acrylate, ethyl p-hydroxybenzoate, N dimethylene phosphoric acid amino maleate, dimethylaminoethyl methacrylate, sulfonated cellulose and sulfonated lignin;
the retarding functional monomer G comprises one or more of glucose, sodium gluconate, white sugar, sodium citrate, tartaric acid, sodium tartrate, sodium hexametaphosphate, sodium pyrophosphate, sodium pentaglycolate and boric acid;
the preservative H is dimethyl fumarate;
the initiator I comprises a composite initiator of ammonium persulfate/sodium bisulfite, ammonium persulfate/hydrogen peroxide, potassium permanganate/oxalic acid and hydrogen peroxide/ascorbic acid;
the chain transfer agent J comprises one or more of thioglycolic acid, mercaptoethanol and sodium methacrylate sulfonate;
the oxidant K comprises one or more of hydrogen peroxide, ammonium persulfate, potassium persulfate, sodium persulfate and potassium permanganate;
the reducing agent L comprises one or more of vitamin C, ferrous sulfate, sodium bisulfite, sodium metabisulfite and sodium hypophosphite;
the alkali liquor M comprises one of sodium hydroxide and potassium hydroxide with the mass concentration of 40%.
2. The method for preparing the general purpose comprehensive type polycarboxylic acid water reducing agent according to claim 1, characterized by: a general comprehensive polycarboxylate superplasticizer is synthesized by adopting multicomponent copolymerization, and the method comprises the following implementation steps: the raw materials comprise the following components in percentage by mass:
1) adding 100 parts of unsaturated polyether macromonomer A and 5-20 parts of starch and modified starch monomer D into a reaction device of a reaction kettle group, adding a tap water purifying agent E80-100 parts, stirring, mixing and dissolving, then sequentially adding 20-60 parts of unsaturated carboxylic acid small monomer B, 0.3-3 parts of an oxidant K, 10-20 parts of a retardation type functional monomer G, 10-20 parts of an anti-mud type functional monomer C, 10-20 parts of a slump-retaining type functional monomer F, 0.1-0.5 part of a reducing agent L, 0.5-3 parts of an initiator I and 0.5-0.8 part of a chain transfer agent J, naturally cooling to 30 ℃ after complete reaction, adding an alkali liquor M, adjusting the pH value to 6-7, and then adding 0.05 part of a preservative H to obtain the universal comprehensive polycarboxylic acid aging water reducer.
Priority Applications (1)
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