Production method of pharmaceutical-grade ferrous sulfate

Embodiment Below in conjunction with accompanying drawing the present invention is described in further detail. This specific embodiment only is an explanation of the invention; it is not a limitation of the present invention; those skilled in the art can make the modification that does not have creative contribution to present embodiment as required after reading this specification sheets, but as long as all are subjected to the protection of patent law in claim scope of the present invention. Embodiment one The production method of the former medicine of ferrous sulfate, its technical process specifically may further comprise the steps as shown in Figure 1: 1., in reactor, add 14 parts of purified water, add sulfuric acid again and regulate ph to 0.3; 2., under agitation, in above-mentioned sulphuric acid soln, add 25 parts in feed grade ferrous sulfate, heating, controlled temperature all dissolves described feed grade ferrous sulfate at 60 ℃; 3., elevated temperature slowly, slowly add 24 parts of technical grade reduced iron powders during to 65 ℃, stirred 1 hour during to 75 ℃, regulate ph to 0.5 with sulfuric acid or iron powder, and control in the described reactor solution density between 1.38～1.40; 4., through step solution 3. with 200 order filter bags and one deck filter paper filtering; 5., will put into retort through step solution 4., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 6., ferrous sulfate crystallization that 5. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 7., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 8., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Embodiment two The production method of the former medicine of ferrous sulfate may further comprise the steps: 1., in reactor, add 16 parts of purified water, add sulfuric acid again and regulate ph to 0.5; 2., under agitation, in above-mentioned sulphuric acid soln, add 27 parts in feed grade ferrous sulfate, heating, controlled temperature all dissolves described feed grade ferrous sulfate at 65 ℃; 3., elevated temperature slowly, slowly add 26 parts of technical grade reduced iron powders during to 75 ℃, stirred 3 hours during to 80 ℃, regulate ph to 1.0 with sulfuric acid or iron powder, and control in the described reactor solution density between 1.38～1.40; 4., through step solution 3. with 200 order filter bags and one deck filter paper filtering; 5., will put into retort through step solution 4., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 6., ferrous sulfate crystallization that 5. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 7., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 8., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Embodiment three The production method of the former medicine of ferrous sulfate may further comprise the steps: 1., in reactor, add 15 parts of purified water, add sulfuric acid again and regulate ph to 0.4; 2., under agitation, in above-mentioned sulphuric acid soln, add 26 parts in feed grade ferrous sulfate, heating, controlled temperature all dissolves described feed grade ferrous sulfate at 65 ℃; 3., elevated temperature slowly, slowly add 25 parts of technical grade reduced iron powders during to 75 ℃, stirred 2 hours during to 80 ℃, regulate ph to 1.0 with sulfuric acid or iron powder, and control in the described reactor solution density between 1.38～1.40; 4., through step solution 3. with 200 order filter bags and one deck filter paper filtering; 5., will put into retort through step solution 4., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 6., ferrous sulfate crystallization that 5. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 7., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 8., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Embodiment four The production method of the former medicine of ferrous sulfate may further comprise the steps: 1., in reactor, add 14～16 parts of purified water, add sulfuric acid again and regulate ph to 0.3～0.5; 2., under agitation, in above-mentioned sulphuric acid soln, add 25～27 parts in feed grade ferrous sulfate, heating, controlled temperature all dissolves described feed grade ferrous sulfate at 60～65 ℃; 3., elevated temperature slowly, slowly add 24～26 parts of technical grade reduced iron powders during to 65～75 ℃, stirred during to 75～80 ℃ 1～3 hour, and regulated ph to 0.5～1.0, and control in the described reactor solution density between 1.38～1.40 with sulfuric acid or iron powder; 4., through step solution 3. with 200 order filter bags and one deck filter paper filtering; 5., will put into retort through step solution 4., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 6., step 5. in, separate out the mother liquor that stays behind the ferrous sulfate crystal and be evacuated to retort, feed in the firm completing steps reactor 3. through following processing back, the ratio control of the solution that makes after the following processing of solution that 3. step is produced and described process is at 0.8 ︰, 1～1 ︰ 0.8, in this step, be treated to below described: in 19 parts of described mother liquors, add sulfuric acid and transfer ph to 0.3～0.5, add 15 parts in feed grade ferrous sulfate again, be heated with stirring to 60 ℃ to all dissolvings, when temperature is risen to 65 ℃, slowly add 14 parts of technical grade reduced iron powders, stirring reaction was 1 hour when temperature was increased to 75 ℃, regulate ph to 0.5, and control in the described retort solution density between 1.38～1.40; 7., ferrous sulfate crystallization that 6. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 8., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 9., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Embodiment five The production method of the former medicine of ferrous sulfate may further comprise the steps: 1., in reactor, add 15 parts of purified water, add sulfuric acid again and regulate ph to 0.3～0.5; 2., under agitation, in above-mentioned sulphuric acid soln, add 26 parts in feed grade ferrous sulfate, heating, controlled temperature all dissolves described feed grade ferrous sulfate at 60～65 ℃; 3., elevated temperature slowly, slowly add 25 parts of technical grade reduced iron powders during to 65～75 ℃, stirred 1～3 hour during to 75～80 ℃, regulate ph to 0.5～1.0 with sulfuric acid or iron powder, and control in the described reactor solution density between 1.38～1.40; 4., through step solution 3. with 200 order filter bags and one deck filter paper filtering; 5., will put into retort through step solution 4., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 6., step 5. in, separate out the mother liquor that stays behind the ferrous sulfate crystal and be evacuated to retort, feed in the firm completing steps reactor 3. through following processing back, 4. and 5. the ratio control of the solution that solution that 3. step is produced and described process are following to be made after handling is at 0.8 ︰, 1～1 ︰ 0.8, proceeds circulation step then; In this step, be treated to below described: in 21 parts of described mother liquors, add sulfuric acid and transfer ph to 0.3～0.5, add 17 parts in feed grade ferrous sulfate again, be heated with stirring to 60 ℃ to all dissolvings, when temperature is risen to 65 ℃, slowly add 16 parts of technical grade reduced iron powders, stirring reaction was 1 hour when temperature was increased to 75 ℃, regulate ph to 0.5, and control in the described retort solution density between 1.38～1.40; 7., ferrous sulfate crystallization that 5. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 8., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 9., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Comparative Examples one The production method of the former medicine of ferrous sulfate, its technical process specifically may further comprise the steps as shown in Figure 2: 1., in reactor, add 14 parts of purified water, add sulfuric acid again and regulate ph to 1.0; 2., under agitation, in above-mentioned sulphuric acid soln, add 25 parts in feed grade ferrous sulfate, heating, controlled temperature is at 60 ℃, described feed grade ferrous sulfate is all dissolved, regulate ph to 0.5, and control in the described reactor solution density between 1.38～1.40 with sulfuric acid or iron powder; 3., through step solution 2. with 200 order filter bags and one deck filter paper filtering; 4., will put into retort through step solution 3., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 5., ferrous sulfate crystallization that 4. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 6., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 7., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Comparative Examples two 1., in reactor, add 16 parts of purified water, add sulfuric acid again and regulate ph to 1.5; 2., under agitation, in above-mentioned sulphuric acid soln, add 27 parts in feed grade ferrous sulfate, heating, controlled temperature is at 70 ℃, described feed grade ferrous sulfate is all dissolved, regulate ph to 1.0, and control in the described reactor solution density between 1.38～1.40 with sulfuric acid or iron powder; 3., through step solution 2. with 200 order filter bags and one deck filter paper filtering; 4., will put into retort through step solution 3., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 5., ferrous sulfate crystallization that 4. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 6., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 7., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Comparative Examples three Before Chinese Pharmacopoeia version promulgation in , the ferrous sulfate production method that our company uses is as follows: 1., in reactor, add 15 parts of purified water, add sulfuric acid again and regulate ph to 1.0; 2., under agitation, in above-mentioned sulphuric acid soln, add 26 parts in feed grade ferrous sulfate, heating, controlled temperature is at 70 ℃, described feed grade ferrous sulfate is all dissolved, regulate ph to 1.0, and control in the described reactor solution density between 1.38～1.40 with sulfuric acid or iron powder; 3., through step solution 2. with 200 order filter bags and one deck filter paper filtering; 4., will put into retort through step solution 3., start stirring, start cooling water circulating device, drop to 25～30 ℃ to temperature, make most of ferrous sulfate crystallization separate out, stop to stir, close cooling water circulation, the ferrous sulfate crystal of separating out is transferred in the crystallizing tank, places more than 2 hours; 5., step 4. in, separate out the mother liquor that stays behind the ferrous sulfate crystal and be evacuated to retort, feed in the firm completing steps reactor 3. through following processing back, the ratio control of the solution that makes after the following processing of solution that 2. step is produced and described process is at 0.8 ︰, 1～1 ︰ 0.8,3. and 4. in this step, continue circulation then and carry out step; Be treated to below described: in 20 parts of described mother liquors, add sulfuric acid and transfer ph to 0.5, add 16 parts in feed grade ferrous sulfate again, be heated with stirring to 70 ℃, and control in the described retort solution density between 1.38～1.40 to all dissolvings; 6., ferrous sulfate crystallization that 4. step is made stirs diffusingly, crystallization is scooped into centrifuge dewatering together with the residue mother liquor; 7., be tiled in the drip pan of baking oven behind the exsiccation, thickness is no more than half of drip pan height, and the control oven temperature is at 35～45 ℃, and the control drying time was at 4～5 hours; 8., abide by the Vibrationsifter standard operating procedure 10 mesh sieves are crossed in the ferrous sulfate crystallization of oven dry. Following table is depicted as the concrete detection data of the product that the embodiment of the invention and Comparative Examples make ? Subsulphate Acidity (PH) Muriate (%) Manganese salt (%) Ferric salt (%) Zinc salt (%) Mercury salt (%) Heavy metal (%) Arsenic salt (%) Content (%) Embodiment one The solution clarification 3.4 0.026 0.08 0.45 0.045 0. 0. 0. 100.5% Embodiment two The solution clarification 3.4 0.026 0.08 0.45 0.045 0. 0. 0. 102.7% Embodiment three The solution clarification 3.4 0.027 0.08 0.45 0.045 0. 0. 0. 103.5% Embodiment four The solution clarification 3.4 0.027 0.08 0.45 0.045 0. 0. 0. 101.6% Embodiment five The solution clarification 3.4 0.026 0.08 0.45 0.045 0. 0. 0. 102．8% Comparative Examples one The solution clarification 3.6 0.03 0.1 0.6 0.08 0. 0. 0. 98.5% Comparative Examples two The solution clarification 3.6 0.03 0.1 0.7 0.085 0. 0. 0. 99.9% Comparative Examples three The solution clarification 3.6 0.03 0.1 0.8 0.09 0.001 0.003 0. 98.5% Last table is described to be the embodiment of the invention and the difference of Comparative Examples on leading indicator, shows in the table, and Comparative Examples is obviously higher than embodiment at manganese salt, ferric salt, zinc salt, mercury salt, heavy metal, arsenic salt, these several respects of content; Purity height, the quality of the product that this explanation use the inventive method makes are good.The pharmaceutical-grade ferrous sulfate of the inventive method preparation meets the relevant regulations of second one of editions Chinese Pharmacopoeia fully.In addition, need to prove that this Comparative Examples is not a production technology commonly used at present, the pharmaceutical-grade ferrous sulfate that its relative prior art is produced also has certain advance.This Comparative Examples is actually the technology that the inventor is developed when the production method of research pharmaceutical-grade ferrous sulfate, although production method is more simple, in the regulation that does not meet second one of editions Chinese Pharmacopoeia aspect some index, as the heavy metal index.