CN1035719C - Apparatus for production of zirconium molybdyl colloid - Google Patents

Abstract

The present invention discloses an apparatus for the production of zirconium-molybdyl colloids for preparing gel-type technetium-99m generators, which comprises a target member cleaning box, a target smashing hammer, a target material dissolving tank, a material solution stirring plate and a colloid generator, wherein a neutralizer is arranged between the dissolving tank and the generator; a high-level tank is used for supplying cleaning solution to the cleaning box; a sample adding bottle and a supply reagent for double connecting balls form the dissolving tank; the neutralizer and the generator are connected with a suction and discharge apparatus composed of a gas bottle, a positive pressure box, a negative pressure box and a mechanical pump; the suction and discharge apparatus is used for the suction, the discharge, and transfer and the pneumatic stir of solution. The apparatus has the advantages of multiple colloid production, high speed, simple, convenient and reliable operation, few dosages of operators and high product quality, and is suitable for bulk production.

Description

Apparatus for production of zirconium molybdyl colloid

The present invention relates to the special-purpose process units of a kind of medical radioisotope.Be a kind of apparatus for production of zirconium molybdyl colloid that is used to prepare gel-type technetium-99m generator specifically.

Molybdic acid zirconium acyl colloid is the intermediate raw material of preparation gel-type technetium-99m generator, to in quartz glass target pipe, take out through the irradiated target material molybdenum trioxide of nuclear reactor, generate alkaline sodium molybdate solution with the lysate dissolution of sodium hydroxide, generate acid molybdic acid zirconium acyl colloid with in the neutralizer salpeter solution and back adding zirconium solution zirconium oxychloride or nitric acid oxidation zirconium again, add an amount of PH regulator solution NaOH again and regulate its pH value, promptly generate medical molybdic acid zirconium acyl colloid.As again this colloid promptly being generated molybdic acid zirconium acyl particle after suction filtration and oven dry processing, with leacheate this particle branch is installed in the glass column, then make medical gel type technetium-99m generator.Technetium-99m ( ^99mTc) be a kind of important medical radioisotope, a kind of radiodiagnosis medicine of Chang Zuowei, it be by its parent molybdenum-99 ( ⁹⁹Mo) decay because molybdenum-99 half life period is short, is 66.02 hours, its daughter technetium-99m half life period is shorter, and only 6.02 hours, so require the production cycle of preparation technetium-99m generator, the generation cycle comprising molybdic acid zirconium acyl colloid is short, to prolong its serviceable life; Because the whole process that molybdic acid zirconium acyl colloid generates all needs carry out, belong to the hot operation again in the hot cell, pollute and to reduce operating personnel's radiation damage particularly important so reduce; Simultaneously also require its product quality to meet the requirement of pharmacopeia as medicinal raw material.In sum, the generation of molybdic acid zirconium acyl colloid need be carried out in the device of a special use, is beneficial to produce in batches.Apparatus for production of zirconium molybdyl colloid commonly used at present as shown in Figure 2; it comprises the target spare Washing cup 1 that is arranged in the hot cell; teflon dissolving cup 2; be provided with the crashing target hammer 4 that is with protection ring 3 in the cup; the colloid that has stirring rod 5 generates cup 6; be fixed in the commentaries on classics sample device 8 on the brandreth 7; the dissolving cup 2 other porcelain dishes 10 that are provided with; be located at the syringe 11 that is connected with commentaries on classics sample device 8 in proparea, hot cell; and application of sample bottle 12, chew on the application of sample bottle 12 with bulbs,double 13 and be connected, chew with emulsion tube down and be connected with valve K1; and add pipe 14 through valve K1 and reagent and is connected, reagent adds manages 14 and stretches in the hot cell.During production, quartz glass target pipe is held under the arm into Washing cup 1, adding pipe 14 by application of sample bottle 12 and reagent joins cleaning fluid in the Washing cup 1 the target pipe is cleaned, to hold under the arm in the dissolving cup 2 through the target pipe after cleaning, and it is smashed with crashing target hammer 4, target material in the target pipe is shed, adding pipe 14 with application of sample bottle 12 and reagent is added to lysate in the dissolving cup 2, target material is dissolved, dissolve and completely add pipe 14 with application of sample bottle 12 and reagent again and neutralizer is added dissolving cup 2 carry out neutralization reaction, adding pipe 14 with application of sample bottle 12 and reagent again joins quantitative zirconium solution in the colloid generation cup 6, and stir, solution after neutralization reaction in the dissolving cup 2 are all transferred in the colloid generation cup 6 that fills zirconium solution with commentaries on classics sample device 8 simultaneously, add pipe 14 with application of sample bottle 12 and reagent again and add the PH regulator solution to dissolving cup 2, rock concussion after several minutes, with changeing sample device 8 this PH regulator solution is transferred in the colloid generation cup 6 again, after fully stirring, generate molybdic acid zirconium acyl colloid.With changeing sample device 8 the molybdic acid zirconium acyl colloid that generates is transferred in the bottle,suction 9, entered suction filtration and baking operation.Pour the broken target pipe in the dissolving cup 2 into porcelain dish 10, operating personnel enter the hot cell and take out above-mentioned each equipment, reload the hot cell after cleaning, and carry out secondary operation production again.Facts have proved, adopt this device to generate molybdic acid zirconium acyl colloid because of being subjected to the restriction of equipment and operational sequence, can only handle two target spares, a collection of target spare will be handled several times just and can finish at every turn, also needs three people's compounding practices, speed of production is slow, efficient is low, and production run moves each equipment, trivial operations, difficulty repeatedly by mechanical arm, sample device transfer solution speed is slow with changeing, even the malfunctioning fault that causes of Chang Yinqi glass piston; After once produce before, the staff need enter the hot cell and take out and reinstall the hot cell after the said equipment cleans to the back zone, hot cell, causes the staff to be subjected to bigger radiation injury; By the Robot actions stirring rod solution that generates is stirred, not only effort is difficult for grasping, and stirs inhomogeneously, directly influences the quality of product.In sum, conventional device is unsuitable for the batch process of molybdic acid zirconium acyl colloid.

The purpose of this invention is to provide a kind of with short production cycle, the efficient height, easy and simple to handle, staff's raying dosage is few, the apparatus for production of zirconium molybdyl colloid of good product quality is produced in batches being adapted to.

The present invention is achieved in that a kind of apparatus for production of zirconium molybdyl colloid, comprise the target piece cleaning box that is arranged in the hot cell, crashing target hammer, target material dissolving tank, broken target pipe is deposited melt pit, material liquid stirring plate and colloid maker, be positioned at the commentaries on classics sample sucking-exhausting device in proparea, hot cell, reagent application of sample bottle and connected bulbs,double, in addition, the proparea, hot cell also is provided with the head tank that cleaning fluid is provided to cleaning case, also be provided with neutralizer between dissolving tank and colloid maker, the neutralizer top is provided with bleeding point, both sides are respectively equipped with inlet and liquid outlet, the top of colloid maker is provided with and takes out/mouth of calming the anger, one side is provided with inlet, opposite side is provided with inlet and colloid floss hole, the inlet of neutralizer is connected with filtrator, liquid outlet is connected with transparent observing pipe and valve, and link to each other with the inlet of colloid maker one side, the inlet and the colloid floss hole of colloid maker opposite side are connected with transparent observing pipe and valve respectively, change the sample sucking-exhausting device and comprise gas cylinder and connected malleation case, and mechanical pump and connected negative pressure box, a bleeding point of the exhausr port of malleation case and negative pressure box is taken out/is calmed the anger switch and links to each other with one, take out/calm the anger taking out/calm the anger and mouthful being connected of switch and colloid maker, the bleeding point of neutralizer is connected with valve, and links to each other with set another bleeding point of negative pressure box.

Compared with prior art, remarkable advantage of the present invention is to abandon the laboratory scale process units of prior art, adopt and produce device in batches, each operation can be dissolved a collection of target material and be generated molybdic acid zirconium acyl colloid in batches, not only speed of production is fast, and it is easy and simple to handle, reliable, the staff is few, raying dosage is little, especially utilize sucking-exhausting device both can implement the malleation discharging under air-proof condition, negative pressure extracting shifts the colloid of intermediate solution or generation, practicable again pneumatic stirring, stir, help improving the quality of product.

Now in conjunction with the accompanying drawings and embodiments the present invention is further described in detail:

Fig. 1 is an apparatus for production of zirconium molybdyl colloid synoptic diagram provided by the present invention, and H represents the hot cell among the figure, and F represents the proparea, hot cell;

Fig. 2 is an apparatus for production of zirconium molybdyl colloid synoptic diagram in the prior art.

As shown in Figure 1, a kind of apparatus for production of zirconium molybdyl colloid comprises the target piece cleaning box 16 that is arranged in the hot cell, stainless steel crashing target hammer 18, stainless steel material liquid stirring plate 19, target material dissolving tank 20, broken target pipe is deposited melt pit 26 and stainless steel colloid maker 24,24 of dissolving tank 20 and colloid makers also are provided with neutralizer 22, the proparea, hot cell is provided with reagent application of sample bottle 33 and connected bulbs,double 34, the head tank 15 of cleaning fluid is provided to cleaning case 16, by gas cylinder 27 and connected malleation case 28, and the commentaries on classics sample sucking-exhausting device of mechanical pump 29 and connected negative pressure box 30 compositions, a bleeding point of the exhausr port of malleation case 28 and negative pressure box 30 is taken out/is calmed the anger switch 31 and links to each other with one, neutralizer 22 tops are provided with bleeding point, both sides are respectively equipped with inlet and liquid outlet, the top of colloid maker 24 is provided with and takes out/mouth 35 of calming the anger, one side is provided with inlet 38, opposite side is provided with inlet 36 and colloid floss hole 37, the inlet of neutralizer 22 is connected with filtrator 21, liquid outlet is connected with transparent observing pipe 23 and valve K4, and link to each other with the inlet 38 of colloid maker 24 1 sides, the inlet 36 of colloid maker 24 opposite sides is connected with valve K7 and transparent observing pipe 39, colloid floss hole 37 also is connected with transparent observing pipe 23 and valve K6, the bleeding point of neutralizer 22 is connected with valve K5, and link to each other with another bleeding point of negative pressure box 30, colloid maker 24 take out/calm the anger mouthfuls 35 with take out/calm the anger switch 31 and link to each other, head tank 15 inner tops are provided with inlet, can adorn cleaning fluid, the bottom is provided with liquid outlet, enter the hot cell by rubber tube and gauge tap K2, be suspended in the top of cleaning case 16, the colloid maker 24 other discharge opeing casees 25, cleaning case 16 of also being provided with, the bottom that broken target pipe is deposited melt pit 26 and discharge opeing case 25 all has discard solution discharge port and is communicated with display pipeline T.

Use this device to carry out target material dissolving and colloid generating run step as follows:

1, produces preparation and close K2, in head tank 15, add the cleaning fluid first water or the redistilled water of capacity; Close K4 and K6, open mechanical pump 29, and will take out/calm the anger switch 31 and place bleed position, open K7 simultaneously, the zirconium solution zirconium oxychloride or the nitric acid oxidation zirconium of quantitatively preparation are drawn in the colloid maker 24, then close K7, open K6, zirconium solution in the colloid maker 24 is carried out pneumatic stirring, make its abundant mixing, close mechanical pump 29 after several minutes;

2, clean the effective well-bucket 17 of quartzy target that the target pipe will be equipped with molybdenum trioxide (MoO) and be transported to the hot cell, put in the cleaning case 16, open K2, the target tube-surface is carried out soaking and washing with head tank 15 interior cleaning fluids;

3, pound the target pipe and all hold under the arm in the dissolving tank 20, they are all smashed, make through irradiated molybdenum trioxide to shed with crashing target hammer 18 cleaning complete quartzy target pipe;

4, the dissolving target material is opened K3, the sodium hydroxide solution of lysate 2mol is added in the dissolving tank 20 with application of sample bottle 33, and stirs the quartz glass fragment with agitating plate 19, and stirring and dissolving liquid quickens the dissolving of molybdenum trioxide, to generate alkaline sodium molybdate solution;

5, neutralization is after molybdenum trioxide all dissolves, filtrator 21 is held under the arm in the dissolving tank 20, close K4, open K5, opening mechanical pump 29 all is drawn into the sodium molybdate solution in the dissolving tank 20 in the neutralizer 22, with application of sample bottle 33 salpeter solution of neutralizer 2mol is added in the dissolving tank 20 again, and the sodium molybdate solutions that are extracted in the neutralizer 22 with meta-alkalescence carry out neutralization reaction, make NaOH reaction excessive in salpeter solution and the sodium molybdate solution generate sodium nitrate and water, the pH value that makes sodium molybdate solution is about 4.0;

6, generate colloid and close K6 and K7, to take out/calm the anger switch 31 and forward bleed position to, open mechanical pump 29, open K4 after about 2 minutes, make through the sodium molybdate solution after the neutralization reaction under stirring condition, all to be pumped in the colloid maker 24, mix the molybdic acid zirconium acyl colloid that generates slant acidity with wherein zirconium solution;

7, transfer pH value after the neutralizer in the dissolving tank 20 is all taken out light, shift out filtrator 21, by application of sample bottle 33 sodium hydroxide solution of PH regulator solution 2mol is joined in the dissolving tank 20, and stir with agitating plate 19, again filtrator 21 is put in the dissolving tank 20 the PH regulator solution in neutralizer 22 is extracted into colloid maker 24, the molybdic acid zirconium acyl colloid of slant acidity is transferred to nearly neutrality, to guarantee the quality of product;

8, K4 is closed in stirring, opens K6, and colloid was proceeded pneumatic stirring about 10 minutes;

9, the discharging colloid is opened gas cylinder 27 to 28 inflations of malleation case, forward the position of calming the anger to taking out/calm the anger switch 31, the sebific duct of the colloid floss hole 37 by being connected in colloid maker 24 ejects the molybdic acid zirconium acyl colloidal pressure that generates, and enters the processing that the suction filtration drying unit carries out subsequent processing.Whether the air valve of regulating gas cylinder 27 is opened the mass rate of emission of controlled amount glue body, can be observed colloid by transparent observing pipe 23 and drained;

10, cleaning the complete back of colloid discharging puts the colloid delivery pipe in the discharge opeing case 25 into, the axle A set around its underpart dissolving tank 20 upwards digs, open running water valve K8, utilize the wash tub pipe 32 usefulness high pressure tap water of front end band nozzle that the quartz chips in the dissolving tank 20 is rushed in melt pit 26, set level dissolving tank 20, in dissolving tank 20, add the first water of capacity with application of sample bottle 33, crashing target hammer 18, agitating plate 19, filtrator 21 is put in the dissolving tank 20 and is cleaned, washing the back takes out, outwell the first water of using, first water with capacity adds in the dissolving tank 20 again, put into filtrator 21, close K4, open K5, open mechanical pump 29, in first water suction neutralizer 22, under pneumatic stirring, clean neutralizer 22, close K5, K6 and K7, turn to bleed position taking out/calm the anger switch 31, open K4, first water in the neutralizer 22 is extracted in the colloid maker 24, close K4, open K7, be drawn into first water to colloid maker 24 again by inlet 36, close K7, open K4 and K6, colloid maker 24 is fully cleaned, close K4 and K7 then with pneumatic stirring, place the position of calming the anger taking out/calm the anger switch 31, cleaning fluid all is pressed into discharge opeing case 25 flows to the display pipeline.

Adopt the required molybdic acid zirconium acyl colloid of 70 gel-type technetium-99m generators of original device production preparation to need 7 hours, 3 people's compounding practices, use device provided by the present invention instead, as long as 1 hour, 1 people operation; The staff needn't enter the hot cell extraction device and clean, so raying dosage is few; It is convenient and reliable to adopt sucking-exhausting device to shift solution, uses pneumatic stirring, and guarantees product quality.

Claims (1)

1. apparatus for production of zirconium molybdyl colloid, comprise the target piece cleaning box (16) that is arranged in the hot cell, crashing target hammer (18), target material dissolving tank (20), broken target pipe is deposited melt pit (26), material liquid stirring plate (19) and colloid maker (24), be positioned at the commentaries on classics sample sucking-exhausting device in proparea, hot cell, reagent application of sample bottle (33) and connected bulbs,double (34), it is characterized in that the proparea, hot cell also is provided with provides head tank (15) from cleaning fluid to target piece cleaning box (16), also be provided with neutralizer (22) between target material dissolving tank (20) and colloid maker (24), neutralizer (22) top is provided with bleeding point, both sides are respectively equipped with inlet and liquid outlet, the top of colloid maker (24) is provided with takes out/calms the anger mouthful (35), one side is provided with inlet (38), opposite side is provided with inlet (36) and colloid floss hole (37), the inlet of neutralizer (22) is connected with filtrator (21), liquid outlet is connected with transparent observing pipe (23) and is connected with valve (K4) and with the inlet (38) of colloid maker (24) one sides, the inlet (36) and the colloid floss hole (37) of colloid maker (24) opposite side are connected with valve (K7 respectively, K6) and transparent observing pipe (39,23), described commentaries on classics sample sucking-exhausting device comprises gas cylinder (27) and connected malleation case (28), and mechanical pump (29) and connected negative pressure box (30), the exhausr port of malleation case (28) is taken out/is calmed the anger switch (31) with the bleeding point of negative pressure box (30) and is connected with one, taking out/calm the anger switch (31) is connected with take out/calm the anger mouthful (35) of colloid maker (24), the bleeding point of neutralizer (24) is connected with valve (K5), and links to each other with set another bleeding point of negative pressure box (30).

Images